HRID2407821

反应详情

EQUATION

反应方程式

HRID 2407821 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirred solution of the compound prepared in Example 425 (0.200 g,) in tetrahydrofuran (4.5 mL) was added zinc dust (0.5782 g), followed by saturated aqueous ammonium chloride (4.5 mL). The mixture was stirred at room temperature for 2 hours. The mixture was diluted with water-ethyl acetate and then filtered through paper. The phases were separated, organic layer dried, concentrated in vacuo and the bright yellow oil purified by column chromatography on silica gel (1-2% methanol in dichloromethane) to provide the title compound (0.132 g) as a yellow oil having the following physical data.

WORKUP

后处理

  1. filtrationfiltered through paper
  2. customThe phases were separated
  3. customorganic layer dried
  4. concentrationconcentrated in vacuo
  5. customthe bright yellow oil purified by column chromatography on silica gel (1-2% methanol in dichloromethane)