HRID2407764

反应详情

EQUATION

反应方程式

HRID 2407764 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of the compound prepared in Example 279 (0.317 g) in N,N-dimethylformamide (6 mL) was added potassium cyanide (0.100 g) at room temperature. The mixture was heated at 80° C. for 18 hours and then cooled to room temperature. The solids were filtered, and the filtrate diluted with ethyl acetate, washed with 1N hydrochloric acid and water. The organic layer was filtered, evaporated in vacuo and purified by column chromatography on silica gel (10-50% ethyl acetate in hexane) to obtain the title compound (0.096 g) having the following physical data.

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. filtrationThe solids were filtered
  3. additionthe filtrate diluted with ethyl acetate
  4. washwashed with 1N hydrochloric acid and water
  5. filtrationThe organic layer was filtered
  6. customevaporated in vacuo
  7. custompurified by column chromatography on silica gel (10-50% ethyl acetate in hexane)