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
- 20 °C
PROCEDURE
实验过程
To a solution of 2-[4-[(1-methylethyl)oxy]-3-(trifluoromethyl)phenyl]-1,3-thiazole (D66) (143 mg) and sodium acetate (82 mg) in acetic acid (5 mL) stirred at 5° C. was added a solution of Br2 (0.026 mL) in acetic acid (1 mL) dropwise. The reaction mixture was stirred at 20° C. until start material was consumed completely. The reaction mixture was basified with 2M NaOH. The resulting solution was diluted with ethyl acetate. The mixture was washed with brine. The organic phase was dried over anhydrous sodium sulphate and evaporated in vacuo. The crude product was purified by column chromatography to give 5-bromo-2-[4-[(1-methylethyl)oxy]-3-(trifluoromethyl)phenyl]-1,3-thiazole (D67) (120 mg). δH (CDCl3, 600 MHz): 1.31 (6H, d), 4.63 (1H, m), 7.05 (1H, d), 7.70 (1H, s), 7.94 (1H, dd), 8.06 (1H, d).
WORKUP
后处理
- customwas consumed completely
- additionThe resulting solution was diluted with ethyl acetate
- washThe mixture was washed with brine
- dry with materialThe organic phase was dried over anhydrous sodium sulphate
- customevaporated in vacuo
- customThe crude product was purified by column chromatography