HRID1443439

反应详情

EQUATION

反应方程式

HRID 1443439 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Compound 50 (200 mg, 0.38 mmol) was dissolved in a mixture of methanol/THF/water, 1:2:1, (20 ml) and cooled on ice-bath. Lithium hydroxide (1.9 ml, 1M) was added slowly. The mixture was stirred for 4 h at 0° C., then neutralized with aqueous acetic acid (20 ml) and extracted with dichloromethane. The organic phase was washed with bicarbonate, water, brine and dried over magnesium sulfate. Purification by chromatography (2% methanol in dichloromethane→4%) gave the title compound as a greyish powder (80%).

WORKUP

后处理

  1. temperaturecooled on ice-bath
  2. extractionextracted with dichloromethane
  3. washThe organic phase was washed with bicarbonate, water, brine
  4. dry with materialdried over magnesium sulfate
  5. customPurification by chromatography (2% methanol in dichloromethane→4%)