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
PROCEDURE
实验过程
A mixture of 100 g (.618 mole) of α,α,α-trifluoro-m-cresol, 106 g (.632 mole) of ethyl bromoacetate, 87.5 g (.632 mole) of potassium carbonate, and 1500 ml of acetone is stirred at reflux for 4 hours, and at room temperature for 18 hours. The mixture is filtered, evaporated under vacuum on a rotorary evaporator at 45° C. and at 85° C. (0.1 mm) to remove excess ethyl bromoacetate. The reaction mixture is taken up in 500 ml of ether, washed three times with 100 ml each of 0.1M potassium carbonate, once with 100 ml of water, 100 ml of 0.01M hydrochloric acid, and 100 ml of water. It is then dried with magnesium sulfate, filtered and evaporated, giving 142 g of the crude product. This is fractionally distilled at 73°-75° C. (0.1 mm) to give 124 g of he purified subject product as a colorless liquid.
WORKUP
后处理
- temperatureat reflux for 4 hours
- filtrationThe mixture is filtered
- customevaporated under vacuum on a rotorary evaporator at 45° C. and at 85° C. (0.1 mm)
- customto remove excess ethyl bromoacetate
- washwashed three times with 100 ml each of 0.1M potassium carbonate
- dry with materialIt is then dried with magnesium sulfate
- filtrationfiltered
- customevaporated