HRID250283

反应详情

EQUATION

反应方程式

HRID 250283 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe mixture is cooled
  2. customthe volatile solvents are evaporated under reduced pressure
  3. washThe basic layer is washed with ether
  4. extractionextracted with ether
  5. dry with materialThe second ether layers are dried over anhydrous magnesium sulfate
  6. concentrationare concentrated
  7. customare crystallized from ether-hexane