反应详情

To 2-(2-(4-(1-hydroxyethyl)-3-(trifluoromethyl)-1H-pyrazol-1-yl)acetamido)-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxamide (1.4 g, 3.36 mmol) in DCM (17 mL) was added a 15 wt % Dess-Martin periodinane in DCM solution (9.51 g, 6.99 mL, 3.36 mmol). The reaction was blanketed with argon and allowed to stir at RT for 6 h. Sodium thiosulfate pentahydrate (5.84 g, 23.53 mmol) was dissolved in water (20 mL) and mixed with saturated aqueous sodium bicarbonate (40 mL) before addition to the reaction mixture. The reaction mixture was allowed to stir for 40 min before the addition of diethyl ether. The aqueous was separated and extracted with diethyl ether (×3). The organics were combined and washed with water (×2) and brine (×1) before drying over MgSO4. The solvent was removed in vacuo to give the title compound as an off white solid (1.2 g, 2.90 mmol, 86%).

1. customThe aqueous was separated
2. extractionextracted with diethyl ether (×3)
3. washwashed with water (×2) and brine (×1)
4. dry with materialbefore drying over MgSO4
5. customThe solvent was removed in vacuo