HRID274419

反应详情

EQUATION

反应方程式

HRID 274419 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

The compound from Step 2 (416 mg) was hydrolysed by dissolving it in THF (4 mL), MeOH (2 mL), and 2N LiOH (1.5 mL). The solution was heated at 70° C. for 5 hours. The mixture was cooled to room temperature, diluted with H2O (50 mL), acidified with glacial acetic acid to pH 5, and diluted with 25% aqueous ammonium acetate (50 mL). The mixture was extracted with ethyl acetate (50 mL), washed with brine (50 mL), dried (MgSO4), and evaporated to dryness to provide the title compound as a white solid; m.p. 173°-175° C.

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. extractionThe mixture was extracted with ethyl acetate (50 mL)
  3. washwashed with brine (50 mL)
  4. dry with materialdried (MgSO4)
  5. customevaporated to dryness