Synthesis of the biologically important dideuterium-labelled adenosine triphosphate analogue ApppI(d₂)

• Petri A. Turhanen

Beilstein J. Org. Chem. 2022, 18, 1466–1470, doi:10.3762/bjoc.18.153

• spectrometry. Keywords: ApppI; ATP; deuterium labelling; HPCCC; mevalonate pathway; NMR; synthesis; Introduction It has become clear and evident that phosphonate chemistry plays a crucial role in drug research and development [1][2][3][4]. There are several phosphonate-containing compounds under research or

• . However, according to the literature, this is the first example reported. The procedure followed for the final synthetic step to ApppI(d2) and the detailed purification method by high-performance counter current chromatography (HPCCC) have previously been described elsewhere [21]. NMR spectroscopic

• salt. This was due to the solvation effect, which had already been reported earlier for the HPCCC purifications of ApppI [21] and ApppD [22]. A typical HPCCC chromatogram for the purification of ApppI(d2) is available in Supporting Information File 1. Conclusion In conclusion, the synthesis of doubly

Synthesis of medronic acid monoesters and their purification by high-performance countercurrent chromatography or by hydroxyapatite

• Elina Puljula,
• Jouko Vepsäläinen and
• Petri A. Turhanen

Beilstein J. Org. Chem. 2016, 12, 2145–2149, doi:10.3762/bjoc.12.204

• monoalkyl esters of medronic acid. Two methods were developed for the purification of medronic acid monoesters: 1) small scale (10–20 mg) purification by using hydroxyapatite and 2) large scale (tested up to 140 mg) purification by high-performance countercurrent chromatography (HPCCC). Keywords

• ]. Countercurrent chromatography (CCC) is an old invention but recently this technique has seen great advances, leading to the appearance of bench top CCC methodology instruments in many laboratories. One of the latest developments in this field is the HPCCC instrument; this achieves improved peak resolution within

• a reasonable time scale [13]. HPCCC relies on the combination of a biphasic immiscible solvent system and a high centrifugal force field. The centrifugal force immobilizes one of the phases in the coiled column (stationary phase), while the remaining phase can be pumped through the column (mobile