HRID1378853

反应详情

EQUATION

反应方程式

HRID 1378853 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3.20 g (5.01 mmol) of the product of Step D dissolved in 5.0 mL of anhydrous THF was added 5.06 mL (5.06 mmol) of a 1.0M solution of tetrabutylammonium fluoride in THF and the reaction mixture was stirred at room temperature under a nitrogen atmosphere. After 2.5 hours 1.0 mL additional tetrabutylammonium fluoride in THF was added and the reaction mixture was stirred for an additional 14 hours. The reaction mixture was then concentrated in vacuo and applied to a silica gel flash chromatography column and eluted with 60% EtOAc-hexane. Combination of the purified fractions and drying in vacuo afforded 0.691 g (26%) of the title compound as an amorphous powder.

WORKUP

后处理

  1. stirringthe reaction mixture was stirred for an additional 14 hours
  2. concentrationThe reaction mixture was then concentrated in vacuo
  3. washeluted with 60% EtOAc-hexane
  4. customCombination of the purified fractions and drying in vacuo