HRID1451133
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
- 100 °C
PROCEDURE
实验过程
--A mixture of salicylic acid (90 g), 2,2,2-trichloroethanoI (270 g) and concentrated sulphuric acid (50 g) was stirred and heated at 100° C. for 4 hours. The mixture was diluted with chloroform (800 ml) and extracted with water (2×500 ml). After further extraction with saturated aqueous sodium bicarbonate solution (1000 ml), the organic layer was washed with water (2×500 ml) and dried (Mg SO4). The chloroform and excess trichloroethanol was removed in vacuo (65° C./20 mmHg) and the product was distilled (110°-112° C./0.5 mmHg) to give 2,2,2-trichloroethyl salicylate (104 g, 59% ) as a clear liquid which solidified on cooling.
WORKUP
后处理
- extractionextracted with water (2×500 ml)
- extractionAfter further extraction with saturated aqueous sodium bicarbonate solution (1000 ml)
- washthe organic layer was washed with water (2×500 ml)
- dry with materialdried (Mg SO4)
- customThe chloroform and excess trichloroethanol was removed in vacuo (65° C./20 mmHg)
- distillationthe product was distilled (110°-112° C./0.5 mmHg)