HRID2407830

反应详情

EQUATION

反应方程式

HRID 2407830 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of the compound prepared in Example 436 (0.053 g) and the compound prepared in Example 214 (0.039 g) in acetonitrile (1 mL) was stirred at room temperature for 30 minutes. Tetramethylammoniumtriacetoxy borohydride (0.094 g) was added and stirring at room temperature continued for 1 hour. The reaction mixture was quenched with aqueous saturated sodium bicarbonate. After stirring at room temperature for 20 minutes, hopeful product was extracted with ethyl acetate, washed with aqueous saturated sodium bicarbonate, dried, evaporated in vacuo to an oil that was purified by column chromatography on silica gel (1-5% methanol in dichloromethane) to provide the title compound (0.008 g) with the following physical data.

WORKUP

后处理

  1. customThe reaction mixture was quenched with aqueous saturated sodium bicarbonate
  2. stirringAfter stirring at room temperature for 20 minutes
  3. extractionhopeful product was extracted with ethyl acetate
  4. washwashed with aqueous saturated sodium bicarbonate
  5. customdried
  6. customevaporated in vacuo to an oil that
  7. customwas purified by column chromatography on silica gel (1-5% methanol in dichloromethane)