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
- 50 °C
PROCEDURE
实验过程
Lithium hydroxide (51 mg) was added at ambient temperature to a solution of 4-[5-(3,5-dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-2-methyl-benzoic acid ethyl ester (0.27 g) (Example I4) in tetrahydrofuran (3 ml) and water (0.75 ml). The reaction mixture was stirred at 50° C. for 18 hours. The reaction mixture was cooled to ambient temperature and diluted with water, acidified by addition of aqueous hydrochloric acid (2M) and extracted three times with ethyl acetate. The combined organic phases were washed with brine, dried over sodium sulfate and concentrated to give 4-[5-(3,5-dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-2-methyl-benzoic acid (0.25 g), which was used without further purification. 1H-NMR (DMSO-d6, 400 MHz): 13.1 (s, 1H), 7.90 (d, 1H), 7.80 (s, 1H), 7.65 (m, 4H), 4.40 (m, 2H), 2.55 (s, 3H).
WORKUP
后处理
- temperatureThe reaction mixture was cooled to ambient temperature
- extractionextracted three times with ethyl acetate
- washThe combined organic phases were washed with brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated