Enabling technologies and green processes in cyclodextrin chemistry

• Giancarlo Cravotto,
• Marina Caporaso,
• Laszlo Jicsinszky and
• Katia Martina

Beilstein J. Org. Chem. 2016, 12, 278–294, doi:10.3762/bjoc.12.30

• -speed ball mills (HSBM), operate in vibrating, mixer or planetary mode. A very simple vibrating BM, consisting of a small milling cup with one or two balls, has been used for a long time in traditional IR spectrometry to homogenize the sample and KBr. Mixer BM are slightly different from the vibrating

Solving the puzzling competition of the thermal C²–C⁶ vs Myers–Saito cyclization of enyne-carbodiimides

• Anup Rana,
• Mehmet Emin Cinar,
• Debabrata Samanta and
• Michael Schmittel

Beilstein J. Org. Chem. 2016, 12, 43–49, doi:10.3762/bjoc.12.6

• , 133.8, 134.1, 135.1, 136.4, 139.3; IR (KBr) : 2976 (w), 2944 (w), 2864 (w), 2825 (w), 2780 (w), 2143 (s, N=C=N), 2123 (s, N=C=N), 1593 (s), 1519 (m), 1488 (s), 1355 (w), 1324 (w), 1284 (w), 1252 (m), 1213 (s), 1034 (m), 908 (s), 822 (m) cm−1; EIMS (70 eV) m/z (%): 289 (29, M+), 288 (99, M+ − H), 274 (54

• , 1H), 7.56 (s, 1H); 13C NMR (100 MHz, CDCl3) δ 21.4, 40.6, 55.8, 73.0, 117.2, 124.3, 125.0, 125.8, 125.8, 126.7, 129.0, 131.0, 132.3, 133.6, 144.3, 145.1, 151.7; IR (KBr) : 2945 (m), 2870 (w), 1630 (m), 1594 (m), 1496 (s), 1488 (s), 1455 (m), 1412 (m), 1343 (s, C-N), 1312 (m), 1296 (w), 1225 (w), 1140

New metathesis catalyst bearing chromanyl moieties at the N-heterocyclic carbene ligand

• Agnieszka Hryniewicka,
• Szymon Suchodolski,
• Agnieszka Wojtkielewicz,
• Jacek W. Morzycki and
• Stanisław Witkowski

Beilstein J. Org. Chem. 2015, 11, 2795–2804, doi:10.3762/bjoc.11.300

• over Na2SO4 and evaporated. The crude product was purified by column chromatography (hexane/ethyl acetate 20:1) to give a yellow solid (1.75 g, 58%). Mp 120–123 °C; IR (KBr) ν: 2977, 2934, 1522, 1368, 1112 cm−1; 1H NMR (400 MHz, CDCl3) δ 2.64 (t, J = 6.8 Hz, 2H, H-4), 2.15 and 2.12 (2s, 9H, H-5a, 7a

• filtrate was extracted with methylene chloride (3 × 20 mL). The organic layers were combined and washed with brine and water, dried over Na2SO4 and evaporated. The crude product was purified by column chromatography (hexane/ethyl acetate 8:1) to give a white solid (660 mg, 50%). Mp 38–40 °C; IR (KBr) ν

• were washed with brine and water, dried over Na2SO4 and evaporated to dryness. After crystallization from ethanol a white solid was obtained (480 mg, 90%). Mp 182–183 °C; IR (KBr) ν: 3369, 2968, 2925, 2779, 1450, 1420, 1265 cm−1; 1H NMR (400 MHz, CDCl3) δ 3.04 (s, 4H, -NCH2CH2N-), 2.64 (t, J = 6.8 Hz

Synthesis and photophysical characteristics of polyfluorene polyrotaxanes

• Aurica Farcas,
• Giulia Tregnago,
• Ana-Maria Resmerita,
• Pierre-Henri Aubert and
• Franco Cacialli

Beilstein J. Org. Chem. 2015, 11, 2677–2688, doi:10.3762/bjoc.11.288

• . The FTIR (KBr pellets) spectra were obtained on a Bruker Vertex 70 spectrophotometer. The molecular weights of copolymers were determined by GPC in THF by using a Water Associates 440 instrument and polystyrene (Pst) calibrating standards. DSC was performed with a Mettler Toledo DSC-12E calorimeter

• , 21H, O(6’)-CH3), 3.19 (dd, J = 3.6 Hz, 7H, C(2)H), 2.10–1.93 (m, Hh), 1.26–1.11 (m, Hi-n), 0.83–0.71 (m, Ho); FTIR (KBr, cm–1): 3433, 2927, 2853, 1724, 1614, 1459, 1410, 1357, 1159, 1091, 1042, 968, 875, 813 cm−1; GPC (THF, Pst standard): Mn = 24300 g·mol−1, Mw/Mn = 1.94. 3·TM-γCD was synthesized by

• –29.20 (Cj–m), 22.59 (Cn), 14.02 (Co); FTIR (KBr, cm–1): 3416, 3058, 2923, 2850, 1634, 1610, 1457, 1405, 1373, 1291, 1095, 888, 810, cm−1; GPC (THF, Pst standard): Mn = 20100 g·mol−1, Mw/Mn = 2.24. Synthesis of the non-rotaxane 3 copolymer: The non-rotaxane copolymer 3 was synthesized under similar

Self-assemblies of γ-CDs with pentablock copolymers PMA-PPO-PEO-PPO-PMA and endcapping via atom transfer radical polymerization of 2-methacryloyloxyethyl phosphorylcholine

• Jing Lin,
• Tao Kong,
• Lin Ye,
• Ai-ying Zhang and
• Zeng-guo Feng

Beilstein J. Org. Chem. 2015, 11, 2267–2277, doi:10.3762/bjoc.11.247

• FTIR spectrometer at room temperature using the KBr pellet method. TGA analysis was performed with using a TA SDT 2960 instrument at a heating rate of 10 °C/min from room temperature to 500 °C in a nitrogen atmosphere. DSC measurements were measured on a SHIMADZU DSC-60 differential scanning

Investigation on the reactivity of α-azidochalcones with carboxylic acids: Formation of α-amido-1,3-diketones and highly substituted 2-(trifluoromethyl)oxazoles

• Kandasamy Rajaguru,
• Arumugam Mariappan,
• Rajendran Suresh,
• Periasamy Manivannan and
• Shanmugam Muthusubramanian

Beilstein J. Org. Chem. 2015, 11, 2021–2028, doi:10.3762/bjoc.11.219

• . Electrospray ionization (ESI) mass spectra were obtained on an LCQ Fleet mass spectrometer, Thermo Fisher Instruments Limited, US and an Agilent mass spectrometer. Infrared spectra were recorded on a Shimadzu FTIR instrument (KBr pellet). Elemental analyses were performed on a Perkin Elmer 2400 Series II

Fe(II)/Et₃N-Relay-catalyzed domino reaction of isoxazoles with imidazolium salts in the synthesis of methyl 4-imidazolylpyrrole-2-carboxylates, its ylide and betaine derivatives

• Ekaterina E. Galenko,
• Olesya A. Tomashenko,
• Alexander F. Khlebnikov,
• Mikhail S. Novikov and
• Taras L. Panikorovskii

Beilstein J. Org. Chem. 2015, 11, 1732–1740, doi:10.3762/bjoc.11.189

• (39.51 ppm). Mass spectra were recorded on a Bruker maXis HRMS–ESI–QTOF, with electrospray ionization in positive mode. IR spectra were recorded on a Bruker FTIR spectrometer Tensor 27 for tablets in KBr, only characteristic absorption is indicated. The single crystal X-ray diffraction experiment was

• ), 118.1(C), 124.2 (CH), 125.6 (CH), 126.6 (C), 127.8 (CH), 127.9 (CH), 128.0 (C), 128.9 (CH), 129.5 (CH), 129.7 (CH), 130.4 (C), 130.6 (C), 133.8 (C), 138.8 (CH), 160.2 (C); HRMS–ESI (m/z): [M – Br]+ calcd for C22Н19ClN3O2, 392.1160; found, 392.1168; IR (KBr, cm−1) ν: 3389, 3042, 1706. General procedure

• ), 139.1 (CH), 160.5 (C); HRMS–ESI (m/z): [M + H]+ calcd for C21Н18N3O2, 344.1394; found, 344.1401; IR (KBr, cm–1) ν: 3124, 2951, 1688. General procedure for the synthesis of pyrrolydes 2 from 5-methoxycarbonylpyrrol-3-ylimidazolium bromides 1. A suspension of 3-(1H-pyrrol)-1H-imidazol-3-ium bromide 1 (1

Reaction of allene esters with Selectfluor/TMSX (X = I, Br, Cl) and Selectfluor/NH₄SCN: Competing oxidative/electrophilic dihalogenation and nucleophilic/conjugate addition

• A. Srinivas Reddy and
• Kenneth K. Laali

Beilstein J. Org. Chem. 2015, 11, 1641–1648, doi:10.3762/bjoc.11.180

• Selectfluor/KBr [13], and the thiocyanation of representative heteroarenes and ketones with NH4SCN [14][15]. Oxidative transformations such as amide to imide mediated by Selectfluor in combination with CuBr have also been shown [16][17]. In an earlier study, we reported on the potential of Selectfluor to act

Consequences of the electronic tuning of latent ruthenium-based olefin metathesis catalysts on their reactivity

• Karolina Żukowska,
• Eva Pump,
• Aleksandra E. Pazio,
• Krzysztof Woźniak,
• Luigi Cavallo and
• Christian Slugovc

Beilstein J. Org. Chem. 2015, 11, 1458–1468, doi:10.3762/bjoc.11.158

• (CD2Cl2) δ 19.0, 20.9, 51.8, 116.1, 117.5, 122.6, 128.1, 129.4, 129.7, 133.9, 134.0, 134.6, 136.2, 138.3, 138.9, 146.8, 155.6, 209.4, 285.5 ppm; IR (KBr) ν: 3320, 3042, 3004, 2949, 2912, 2855, 2837, 2810, 2237, 1959, 1704, 1682, 1601, 1586, 1556, 1478, 1454, 1445, 1427, 1418, 1398, 1378, 1326, 1315, 1289

• , 117.0, 122.8, 129.2, 130.8, 133.4, 134.3, 136.0, 138.9, 139.0, 145.9, 152.2, 156.3, 190.0, 210.6, 288.2 ppm; IR (KBr) ν: 3003, 2952, 2912, 2854, 2734, 2232, 1950, 1734, 1694, 1605, 1584, 1551, 1480, 1419, 1401, 1379, 1319, 1294, 1261, 1222, 1174, 1154, 1138, 1092, 1036, 987, 929, 910, 887, 846, 813, 794

New depsidones and isoindolinones from the mangrove endophytic fungus Meyerozyma guilliermondii (HZ-Y₂) isolated from the South China Sea

• Senhua Chen,
• Zhaoming Liu,
• Yayue Liu,
• Yongjun Lu,
• Lei He and
• Zhigang She

Beilstein J. Org. Chem. 2015, 11, 1187–1193, doi:10.3762/bjoc.11.133

• /δH 2.05 for acetone-d6), and coupling constants (J) are given in Hz. UV data were measured on a PERSEE TU-1900 spectrophotometer. IR spectra were measured on a Nicolet Nexus 670 spectrophotometer, in KBr discs. EIMS on a DSQ EI-mass spectrometer (Thermo, Shanghai, China) and HREIMS data were measured

• ): white amorphous powder; UV (MeOH) λmax (log ε): 262 (4.25), 364 (3.56) nm; IR (KBr) νmax: 3426, 2922, 2853, 1680, 1620, 1506, 1458, 1383, 1265, 1193, 1074, 908, 877, 809 cm−1; EIMS (m/z): 288; HREIMS (m/z): 288.0627 (calcd for C15H12O6, 288.0628); 1H NMR (CD3OD, 500 MHz) and 13C NMR (CD3OD, 125 MHz

• ), see Table 1. Botryorhodine F (2): white amorphous powder; UV (MeOH) λmax (log ε): 262 (4.25), 364 (3.56) nm; IR (KBr) νmax: 3426, 2922, 2853, 1686, 1620, 1587, 1458, 1357, 1284, 1193, 1155, 1074, 915, 875, 812 cm−1; EIMS (m/z): 302; HREIMS (m/z): 302.0787 (calcd for C16H14O6, 302.0785); 1H NMR (CD3OD

New palladium–oxazoline complexes: Synthesis and evaluation of the optical properties and the catalytic power during the oxidation of textile dyes

• Rym Hassani,
• Mahjoub Jabli,
• Yakdhane Kacem,
• Jérôme Marrot,
• Damien Prim and
• Béchir Ben Hassine

Beilstein J. Org. Chem. 2015, 11, 1175–1186, doi:10.3762/bjoc.11.132

• , 70.2, 68.0, 31.3, 18.5, 15.9; 31P NMR (MeOD, 75 MHz) δ 36.0 ppm; TOF–MS (ES+) for (C34H31NOPPd): theoretical [M − Cl]+: 602.1199; measured [M − Cl]+: 602.1201; FTIR (KBr pellets, cm−1): 2956.7, 1637.4, 1436.7, 1201.0, 1094.9, 1011.0, 692.3, 513.4. Synthesis of dichloro-[1,2-bis((S)-4-phenyl-4,5

• , 130.7, 130.0, 128.2, 127.1, 126.4, 125.8, 124.6, 124.2, 70.8, 69.3, 30.0, 19.1, 15.3; TOF–MS (ES+) for (C18H29ClN4O2Pd): theoretical [M − Cl]+: 615.1365; measured [M − Cl]+: 615.1361; FTIR (KBr pellets, cm−1): 2957.8, 1642.2, 1377.8, 1200.4, 1030.8, 776.0, 573. Complex 12: [α]D −5.7 ± 0.5 (c 0.94, CHCl3

• ; FTIR (KBr pellets, cm−1): 2963.9, 2250.8, 1635.4, 1545.2, 1260.3, 1018.8. Oxidative degradation procedures of dyes All experiments were carried out in a batch system for a period of time (sufficient to achieve equilibrium) and were uniformly agitated at a speed of 150 rpm. The pH of the solution was

Reactions of nitroxides 15. Cinnamates bearing a nitroxyl moiety synthesized using a Mizoroki–Heck cross-coupling reaction

• Jerzy Zakrzewski and
• Bogumiła Huras

Beilstein J. Org. Chem. 2015, 11, 1155–1162, doi:10.3762/bjoc.11.130

• ) 20.87 (2×CH3), 31.67 (2×CH3), 43.87 (2×CH2), 60.46 (2×C(CH3)2), 66.76 (CH-O-), 118.51 (CH), 128.30 (CH), 129.10 (CH), 130.52 (CH), 134.57 (C), 145.00 (CH), 166.68 (C=O); IR (cm−1, KBr) 2976, 2937, 1712, 1639, 1450, 1308, 1168, 1008, 978, 859, 765, 709, 685. 2,2,6,6-Tetramethyl-1-oxyl-4-piperidyl 3-E-(4

• −1, KBr) 2975, 1706, 1638, 1474, 1319, 1267, 1173, 1150, 1206, 979, 822. 2,2,6,6-Tetramethyl-1-oxyl-4-piperidyl 3-E-(4-methoxyphenyl)acrylate (5d) 75.8%; mp 70–74 °C; MS (EI, 70 eV, m/z, int [%]) 332 (19, M+), 302 (6), 284 (2), 267 (5), 246 (4), 178 (32), 161 (100, ArCH=CHCO), 154 (20), 140 (8), 139

• (d, J = 16.0 Hz, 1H, Ar-CH=CH-COO); 13C NMR (50 MHz, δ, CDCl3, TMS, PhNHNH2) 20.79 (2×CH3), 31.96 (2×CH3), 44.12 (2×CH2), 55.57 (OCH3), 59.90 (2×C(CH3)2), 66.68 (CH-O-), 114.51 (CH), 116.03 (CH), 127.33, 129.94 (CH), 144.60 (CH), 161.57, 167.02 (C=O); IR (cm−1, KBr) 1707, 1632, 1604, 1515, 1290, 1255

Synthesis of photoresponsive cholesterol-based azobenzene organogels: dependence on different spacer lengths

• Yuchun Ren,
• Bin Wang and
• Xiuqing Zhang

Beilstein J. Org. Chem. 2015, 11, 1089–1095, doi:10.3762/bjoc.11.122

• spectroscopy (IR) was measured on a Nicolet 6700 spectrometer from 4000 to 500 cm−1 at room temperature. The samples were prepared as KBr pellets. The morphology of the gel samples were examined by scanning electron microscopy (SEM, S5200, FEI Company) under an acceleration voltage of 30 kV. UV–vis absorption

Indolizines and pyrrolo[1,2-c]pyrimidines decorated with a pyrimidine and a pyridine unit respectively

• Marcel Mirel Popa,
• Emilian Georgescu,
• Mino R. Caira,
• Florentina Georgescu,
• Constantin Draghici,
• Raluca Stan,
• Calin Deleanu and
• Florea Dumitrascu

Beilstein J. Org. Chem. 2015, 11, 1079–1088, doi:10.3762/bjoc.11.121

• spectra (for representative compounds) were recorded on a Bruker Vertex 70 spectrometer with horizontal device for attenuated reflectance and diamond crystal, in a spectral window ranging from 4000 to 400 cm−1 or on a Nicolet Impact 410 Spectrometer in KBr pellets. Elemental analysis was performed on a

• , 168.5 (C-4, C-1’, C-1”), 135.7 (C-4”), 139.2 (C-5’), 151.5 (C-3’), 154.7 (C-6), 155.3 (C-2), 190.7 (COAr); IR (KBr, cm−1): 1696, 1627, 1550, 1450, 1341, 1213. General procedure for obtaining pyrrolo[1,2-c]pyrimidines 12a–h 4-(2-Pyridyl)pyrimidinium bromide (3 mmol) 11a–e previously obtained and

• (C-5’), 120.6 (C-8), 126.8 (C-7), 128.8 (C-5), 129.3 (C-2), 131.4 (J = 8.9 Hz, C-2”, C-6”), 122.8, 126.1, 135.7, 139.5, 160.9 (C-3, C-8a, C-6, C-4’, C-1”), 157.9 (C-6’), 159.4 (C-2’), 165.1 (J = 252.3 Hz, C-4”), 184.3 (COAr), 193.1 (CO); IR (KBr, cm−1): 1659, 1630, 1581, 1510, 1485, 1431, 1359, 1213

Chiroptical properties of 1,3-diphenylallene-anchored tetrathiafulvalene and its polymer synthesis

• Masashi Hasegawa,
• Junta Endo,
• Seiya Iwata,
• Toshiaki Shimasaki and
• Yasuhiro Mazaki

Beilstein J. Org. Chem. 2015, 11, 972–979, doi:10.3762/bjoc.11.109

• ), 2.44 (s, 6H), 2.43 (s, 6H), 1.19 (t, J = 6.8 Hz, 12H); 13C NMR (100 MHz, CDCl3) δ 204.2, 136.9, 136.0, 130.8, 127.8, 127.7, 126.7, 126.6, 117.4, 114.8, 112.8, 107.3, 28.7, 22.8, 22.5, 19.4; IR (KBr): 2958, 2918, 2866, 1914, 1568, 1499, 1418, 835, 759 cm−1; anal. calcd for C37H36S12: C, 51.35; H, 4.19

Synthesis and characterization of the cyanobenzene-ethylenedithio-TTF donor

• Sandrina Oliveira,
• Dulce Belo,
• Isabel C. Santos,
• Sandra Rabaça and
• Manuel Almeida

Beilstein J. Org. Chem. 2015, 11, 951–956, doi:10.3762/bjoc.11.106

• ,), 7.38 (dd, J = 1, 8.1 Hz, 1H,), 7.31 (d, J = 8.1 Hz, 1H), 3.32 (s, 4H); 13C NMR (CD3)2SO) 142.8, 138.1, 130.9, 126.3, 123.9, 118.7, 113.44, 109.73, 30.11; υmax (KBr)/cm−1: 3062 (m, Ar-H), 2922 (s, CH2), 2229 (s, C≡N), 1637 and 1446 (m, C=C), and 582 (m, C-S); UV–vis (DCM) λmax = 231 nm. Crystal

Trifluoromethyl-substituted tetrathiafulvalenes

• Olivier Jeannin,
• Frédéric Barrière and
• Marc Fourmigué

Beilstein J. Org. Chem. 2015, 11, 647–658, doi:10.3762/bjoc.11.73

• for 15 days to produce thin needles which were filtered and recrystallized by slow evaporation in CH3CN to give the title compound as elongated black plates (20 mg, 78%); Anal. calcd for C30H14F6N4S12: C, 38.78; H, 1.52; N, 6.03; found: C, 38.61; H, 1.51; N, 6.08; IR νCN (KBr): 2222 cm−1. Preparation

TTFs nonsymmetrically fused with alkylthiophenic moieties

• Rafaela A. L. Silva,
• Bruno J. C. Vieira,
• Marta M. Andrade,
• Isabel C. Santos,
• Sandra Rabaça,
• Dulce Belo and
• Manuel Almeida

Beilstein J. Org. Chem. 2015, 11, 628–637, doi:10.3762/bjoc.11.71

• CH2Cl2 (Rf = 0.47). Single crystals were obtained by slow evaporation of a chloroform solution of 1. Yield: 28% (176 mg); Anal. calcd for C18H18N2S7: C, 44.41; H, 3.72; N, 5.75; S, 46.11; found: C, 44.53; H, 4.00; N, 5.17; S, 46.33; FTIR (KBr): 2960 (m, –CH2–), 2252 (m, –C≡N), 1634 (m, C=C), 1423 (S, S

• , 2.89; N, 5.97; S, 51.07; FTIR (KBr) 2924 (m, –CH2–), 2251 (m, –C≡N), 1654 and 1421 (m, C=C), 1425 (S, S–CH2–R) cm−1; 1H NMR (300 MHz, CDCl3) δ 7.26 (s, 1H, –C=CH–C–), 3.10 (t, J = 7.15 Hz, 4H, S–CH2–CH2–CN), 2.74 (t, J = 6.95 Hz, 4H, S–CH2–CH2–CN), 1.55 (s, 3H, C–CH3), 13C NMR (100 MHz CD2Cl2) δ 144.49

Synthesis of 1,2-cis-2-C-branched aryl-C-glucosides via desulfurization of carbohydrate based hemithioacetals

• Henok H. Kinfe,
• Fanuel M. Mebrahtu,
• Mandlenkosi M. Manana,
• Kagiso Madumo and
• Mokela S. Sokamisa

Beilstein J. Org. Chem. 2015, 11, 583–588, doi:10.3762/bjoc.11.64

• for the enzymes of Mycobacterium tuberculosis, in particular a deacetylase implicated in the biosynthesis of mycothiol, is under way and the results will be reported in the future. Single X-ray crystal structure of hemithioacetal 3a. (i) CAN, wet silica, KBr, CH2Cl2/CH3CN (1:1), rt, 30 min; (ii) a

Hetero-Diels–Alder reactions of hetaryl and aryl thioketones with acetylenic dienophiles

• Grzegorz Mlostoń,
• Paulina Grzelak,
• Maciej Mikina,
• Anthony Linden and
• Heinz Heimgartner

Beilstein J. Org. Chem. 2015, 11, 576–582, doi:10.3762/bjoc.11.63

• information: Melting points were determined in capillaries using a MEL-TEMP II apparatus (Aldrich) and are uncorrected. IR spectra were recorded with a FTIR NEXUS spectrophotometer as KBr pellets; absorptions (ν) in cm−1. 1H and 13C NMR spectra were measured on a Bruker Avance III (1H at 600 and 13C at 150

• [4,5]cyclohepta[1,2,3-ij]isothiochromene-6,7-dicarboxylate (4b): Yield: 328.5 mg (90%). Colorless crystals; mp 147.5–148.0 °C (MeOH); IR (KBr) ν: 3061 (w), 2948 (w), 1732 (s), 1725 (s), 1597 (w), 1562 (w), 1435 (m), 1270 (s), 1232 (s), 1030 (w), 751(m) cm−1; 1H NMR (600 MHz, CDCl3) δ 7.61 (d, J = 12 Hz

• ]isothiochromene-6,7-dicarboxylate (4c): Yield: 83 mg (46%). Orange solid; mp 139.7–140.0 °C (purified chromatographically); IR (KBr) ν: 3018 (w), 2947 (w), 1728 (s), 1725 (s), 1596 (w), 1563 (w), 1433 (w), 1264 (s),1229 (s), 1097 (w), 771 (w) cm−1; 1H NMR (600 MHz, CDCl3) δ 7.77 (d, J = 6 Hz, 1Harom), 7.49–7.45

An unusually stable chlorophosphite: What makes BIFOP–Cl so robust against hydrolysis?

• Roberto Blanco Trillo,
• Jörg M. Neudörfl and
• Bernd Goldfuss

Beilstein J. Org. Chem. 2015, 11, 313–322, doi:10.3762/bjoc.11.36

• Hz, 1H), 6.99 (t, J = 9 Hz, 1H), 7.09 (d, J = 6 Hz, 1H), 7.19 (d, J = 6 Hz, 1H); 13C NMR (75 MHz, CDCl3) δ 15.63, 15.90, 21.76, 22.23, 22.61, 25.86, 27.09, 32.72, 33.04, 35.68, 38.20, 38.33, 42.61, 42.72, 47.65, 47.81, 118.62, 120.29, 121.47, 121.86, 126.86, 127.40, 127.91, 134.34, 134.69; IR (KBr) ν

Novel biphenyl-substituted 1,2,4-oxadiazole ferroelectric liquid crystals: synthesis and characterization

• Mahabaleshwara Subrao,
• Dakshina Murthy Potukuchi,
• Girish Sharada Ramachandra,
• Poornima Bhagavath,
• Sangeetha G. Bhat and
• Srinivasulu Maddasani

Beilstein J. Org. Chem. 2015, 11, 233–241, doi:10.3762/bjoc.11.26

• the KBr pellet method. 1H and 13C NMR spectra are recorded on Bruker NMR (400 MHz) spectrometers using CDCl3 as solvent. Elemental analyses are carried out using an Elementar vario MICRO cube. Polarization exhibited by tilted LC phase structures is determined by field reversal method. (a) Focal conic

A one-pot multistep cyclization yielding thiadiazoloimidazole derivatives

• Debabrata Samanta,
• Anup Rana,
• Jan W. Bats and
• Michael Schmittel

Beilstein J. Org. Chem. 2014, 10, 2989–2996, doi:10.3762/bjoc.10.317

• -phenylthiourea) (1a) matched with those of a literature report [17]. 1,1'-(1,2-Phenylene)bis(3-benzylthiourea) (1b) White solid: mp = 159 °C, 86% yield (6.51 g, 15.9 mmol); IR (KBr) : 3233, 3186, 3031, 1535, 1344, 1309, 1114, 969, 848, 698 cm−1; 1H NMR (400 MHz, DMSO-d6) δ 4.69 (d, 3J = 3.8 Hz, 4H, 4-H), 7.22

• ; N, 13.68; S, 16.06. 1,1'-(1,2-Phenylene)bis(3-cyclohexylthiourea) (1c) White solid: mp = 185 °C, 95% yield (6.85 g, 17.6 mmol); IR (KBr) : 3333, 3262, 3138, 2930, 2851, 1548, 1395, 1385, 1260, 1192, 982, 893, 784, 755, 623, 537 cm−1; 1H NMR (400 MHz, DMSO-d6) δ 1.11–1.32 (m, 10H, 1eq, 2eq, 3eq, 10

• , dichloromethane, Rf = 0.62; yellow solid: mp = 170 °C, 68% yield (582 mg, 1.70 mmol); IR (KBr) : 3028, 1919, 1883, 1835, 1752, 1662, 1588, 1548, 1489, 1449, 1404, 1289, 1218, 1148, 1104, 1069, 1027, 1000, 915, 873, 741 cm−1; 1H NMR (400 MHz, CD2Cl2) δ 7.17–7.21 (m, 3H, 3, 10-H), 7.24–7.31 (m, 2H, 1, 5 or 6-H

Preparation and evaluation of cyclodextrin polypseudorotaxane with PEGylated liposome as a sustained release drug carrier

• Kayoko Hayashida,
• Taishi Higashi,
• Daichi Kono,
• Keiichi Motoyama,
• Koki Wada and
• Hidetoshi Arima

Beilstein J. Org. Chem. 2014, 10, 2756–2764, doi:10.3762/bjoc.10.292

• , Worcestershire, UK). The dynamic light scattering was analyzed by the general purpose mode. The measurements were carried out at least in triplicates. FTIR The sample preparation was performed by using the KBr method. The FTIR spectrum of γ-CD PPRX with DOX/PEG-LP was recorded on a JIR-6500W FTIR spectrometer

Synthesis of nanodiamond derivatives carrying amino functions and quantification by a modified Kaiser test

• Gerald Jarre,
• Steffen Heyer,
• Elisabeth Memmel,
• Thomas Meinhardt and
• Anke Krueger

Beilstein J. Org. Chem. 2014, 10, 2729–2737, doi:10.3762/bjoc.10.288

• (max. 80 W, 35 kHz), centrifuges: Hettich EBA 21 Type 1004, FTIR: Perkin-Elmer 1600 Series with ATR equipment and home-made vacuum cell (KBr pellet). Samples for measurements using the vacuum cell were heated at 100–120 °C for 2 h in vacuo in order to remove most of the water adsorbed on the diamond