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
A solution of 3-(2′,4′,5′-trifluoro-biphenyl-4-yloxymethyl)-benzoic acid methyl ester (18.96 g, 50.92 mmol) in inhibitor free THF (100 mL) was treated with a near solution of lithium hydroxide monohydrate (8.4 g, 200.2 mmol) in water (100 mL) at room temperature and heated at 60° C. for 4 h. The reaction mixture was cooled, diluted with water, acidified with aq. 2N HCl and extracted with ethyl acetate. The organic layers were combined, washed with 1/1 water/brine, brine, dried (MgSO4), filtered and concentrated to give 3-(2′,4′,5′-trifluoro-biphenyl-4-yloxymethyl)-benzoic acid (17.89 g, 98.0%) as an off white solid. LC-MS (ES) calculated for C20H13F3O3, 358.32; found m/z 357 [M−H]−.
WORKUP
后处理
- temperatureThe reaction mixture was cooled
- extractionextracted with ethyl acetate
- washwashed with 1/1 water/brine, brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated