反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
345 mg (0.97 mmol) of ethyl 2-(bromomethyl)-4-(2-chlorophenyl)pyrimidine-5-carboxylate were added to a solution of 200 mg (1.45 mmol) of trifluoromethyltetrazole in 10 ml of acetonitrile. Then 174 mg (1.26 mmol) of potassium carbonate were added to the reaction solution, and the mixture was stirred at 60° C. for 6 hours. After cooling to room temperature, the reaction solution was filtered and the mother liquor was freed from the solvent under reduced pressure. 10 ml of water were added to the residue and the mixture was extracted with ethyl acetate (3×20 ml). The combined organic phases were dried over sodium sulphate. The solvent was removed under reduced pressure and the residue was purified by chromatography. (logP: 3.56; MH+: 413; 1H-NMR (400 MHz, DMSO, ppm): 0.99 (t, 3H), 4.13 (q, 2H), 6.62 (s, 2H), 7.50 (m, 4H), 9.28 (s, 1H).
WORKUP
后处理
- temperatureAfter cooling to room temperature
- filtrationthe reaction solution was filtered
- addition10 ml of water were added to the residue
- extractionthe mixture was extracted with ethyl acetate (3×20 ml)
- dry with materialThe combined organic phases were dried over sodium sulphate
- customThe solvent was removed under reduced pressure
- customthe residue was purified by chromatography