HRID446520

反应详情

EQUATION

反应方程式

HRID 446520 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The compound (135 mg, 0.289 mmol) obtained in Example 4g and the compound (103 mg, 0.473 mmol) obtained in Example 18a were dissolved in methylene chloride (4 mL), acetic acid (73 μL) and sodium triacetoxyborohydride (137 mg, 0.645 mmol) were added, and the mixture was stirred overnight at room temperature. Sodium borohydride (16 mg, 0.430 mmol) was added, and the mixture was stirred at room temperature for 20 minutes. The solvent was evaporated under reduced pressure, and the resulting residue was purified by NH silica gel column chromatography (hexane:ethyl acetate=1:1→1:2, v/v) to give the title compound (114 mg; yield, 40%) as a white solid.

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature for 20 minutes
  2. customThe solvent was evaporated under reduced pressure
  3. customthe resulting residue was purified by NH silica gel column chromatography (hexane:ethyl acetate=1:1→1:2, v/v)