HCID 68157700, compound → HCID 178498688, compound

Participants

Reaction Steps

A solution of 3-cyclopropyl-5-fluoro-2-{(S)-1-[9-(tetrahydro-pyran-2-yl)-9H-purin-6-ylamino]ethyl}-3H-benzoimidazole-4-carboxylic acid methyl ester (178 mg, 0.37 mmol) in DCM was loaded onto an Isolute® SCX-2 cartridge which was washed with MeOH followed by 2M NH3/MeOH. The basic fractions were combined, concentrated in vacuo and the resulting residue subjected to a second SCX-2 cartridge purification. The basic fractions were combined, concentrated in vacuo and the resulting residue purified by column chromatography (Si—PCC, gradient 0-10% MeOH in DCM) to afford 386 as a white solid (36 mg, 25%). LCMS (Method K): RT 3.03 min [M+H]+ 396.04. 1H NMR (DMSO-d6, 400 MHz): δ 8.25-8.11 (2H, m), 8.03 (1H, s), 7.73 (1H, dd, J=8.81, 4.72 Hz), 7.13 (1H, t, J=9.78 Hz), 5.98 (1H, s), 3.94 (3H, s), 1.68 (3H, d, J=6.74 Hz), 1.17-0.84 (4H, m)

Provenance & Evidence