反应详情

To a solution of [4-(trifluoromethyl)pyridin-2-yl]methanol (340 mg, 1.9 mmol) in DMF (10 mL) was added sodium hydride (150 mg, 3.8 mmol). After being stirred at room temperature for 5 min. 1,1-dimethylethyl bromoacetate (0.28 mL, 1.9 mmol) was added. Stirring was continued at room temperature for 1 h. Water (20 mL) was added and the resulting solution was extracted with EtOAc. The water layer was neutralized to pH=5 with HCl and extracted with EtOAc twice. The combined organic layers were dried (MgSO4) and concentrated under vacuum to give the title compound which was used for the next reaction without purification. MS (M+H) 292.2.

1. stirringStirring
2. waitwas continued at room temperature for 1 h
3. extractionthe resulting solution was extracted with EtOAc
4. extractionextracted with EtOAc twice
5. dry with materialThe combined organic layers were dried (MgSO4)
6. concentrationconcentrated under vacuum