HRID266590
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
Sodium hydride (1.05 g of 80% powder) was suspended in THF and to this was added a solution of 2.2,2-trifluoroethanol (1.9 g) in THF, followed by a solution of 4-chloro-3-fluoro-2-methylsulphonylbenzoic acid (4 g) in THF. The resultant mixture was stirred for 2 hours and then acidified with 2M HCl. The mixture was extracted with ether, washed with water, dried (anhydrous magnesium sulphate) and filtered. The filtrate was evaporated to dryness yielding 4-chloro-2-methylsulphonyl-3-(2,2,2-trifluoroethoxy)benzoic acid (5.26 g) as a whim solid, NMR (DMSO d6) 2.5(s,3H), 4.8(q,2H), 7.5(d, 1H), 8.0(d, 1H).
WORKUP
后处理
- extractionThe mixture was extracted with ether
- washwashed with water
- dry with materialdried (anhydrous magnesium sulphate)
- filtrationfiltered
- customThe filtrate was evaporated to dryness