Sodium sulfate decahydrate → HCID 66589110, compound

Participants

Reaction Steps

A solution of ethyl 9-(5-cyclopropyl-1H-pyrazol-3-yl)-2-[(S)-1-(4-fluorophenyl)ethylamino]-9H-purine-6-carboxylate (Example 11; 0.03 g, 0.069 mmol) in THF (3 ml) was cooled to 0° C. To which was slowly added lithium aluminium hydride (1.0 M in THF, 0.076 ml, 1.1 eq.). The reaction mixture was stirred at 0° C. for 30 minutes, at which point sodium sulfate decahydrate was added until bubbling stopped. The reaction was then filtered through a plug of celite, washed with THF (3×30 ml), and concentrated. The resulting residue was purified by column chromatography (DCM:MeOH=15:1) to give the title compound (0.09 g, 33%). NMR (400 MHz, CDCl3) 8.27 (s, 1H), 7.39-7.36 (m, 2H), 7.03-6.98 (m, 2H), 6.32 (s, 1H), 5.65-5.64 (m, 1H), 5.10-5.07 (m, 1H), 5.03 (s, 2H), 3.87-3.85 (m, 1H), 1.93-1.88 (m, 1H), 1.57 (d, J=6.8 Hz, 3H), 1.08-1.06 (m, 2H), 0.81-0.77 (m, 2H). MS: Calcd.: 393; Found: [M+H]+ 394.

Provenance & Evidence