HRID250283
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
- 85 °C
PROCEDURE
实验过程
A mixture of 6-{4-[3-(2,6-dichloro-phenyl)-5-isopropyl-isoxazol-4-ylmethoxy]-2-methyl-phenyl}-1H-indole-3-carboxylic acid methyl ester (80 mg, 0.15 mmol), 5 N sodium hydroxide (150 μL, 0.750 mmol), methanol (2 mL) and THF (1 mL) is heated at 85° C. for five hours. The mixture is cooled and 5 mL of water is added and the volatile solvents are evaporated under reduced pressure. The basic layer is washed with ether and then acidified with 1 N HCl and extracted with ether. The second ether layers are dried over anhydrous magnesium sulfate, are concentrated, and are crystallized from ether-hexane to provide 42 mg (54%) of the title compound. LC-ES/MS m/e 535.0 (M+1), 93.2% purity.
WORKUP
后处理
- temperatureThe mixture is cooled
- customthe volatile solvents are evaporated under reduced pressure
- washThe basic layer is washed with ether
- extractionextracted with ether
- dry with materialThe second ether layers are dried over anhydrous magnesium sulfate
- concentrationare concentrated
- customare crystallized from ether-hexane