反应详情

To a solution of ethyl 2-(4-(benzyloxy)-2-(1H-pyrazol-1-yl)pyrimidin-5-yl)acetate, 12-b, (90 mg, 0.27 mmol) in TRF (6 ml) was added LiOH monohydrate (19 mg, 0.8 mmol) in H2O (3 ml). The mixture was stirred at room temperature for 3 hours. The mixture was concentrated under vacuum and the remaining aqueous solution was extracted with ethyl acetate (5 ml). The separated aqueous phase was adjusted to pH=2 with Conc. HCl. The solid crashed out and was filtered to give compound 12-c (40 mg, 48.5%). 1HNMR (DMSO-d6, 300 MHz): δ 12.56 (s, 1H), 8.66 (s, 1H), 8.47 (s, 1H), 7.84 (s, 1H), 7.32-7.52 (M, 5H), 6.59 (s, 1H), 5.57 (S, 2H), 3.61 (s, 2H). (M+H)+=311.1.

1. concentrationThe mixture was concentrated under vacuum
2. extractionthe remaining aqueous solution was extracted with ethyl acetate (5 ml)
3. filtrationwas filtered