HRID2407765

反应详情

EQUATION

反应方程式

HRID 2407765 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a suspension of the compound prepared in Example 280 (0.672 g) in hydrochloric acid (2.3 mL) and methanol (7 mL) was added portionwise iron (0.680 g) slowly. After addition was complete, the mixture was stirred at room temperature for 1 hour. The mixture was evaporated in vacuo, diluted with dichloromethane, filtered, and purified by column chromatography on silica gel (5-70% ethyl acetate in hexane) to obtain the title compound (0.460 g) having the following physical data.

WORKUP

后处理

  1. additionAfter addition
  2. customThe mixture was evaporated in vacuo
  3. additiondiluted with dichloromethane
  4. filtrationfiltered
  5. custompurified by column chromatography on silica gel (5-70% ethyl acetate in hexane)