HRID433045

反应详情

EQUATION

反应方程式

HRID 433045 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Triphenylphosphine (7.92 g, 30 mmol) in THF (40 ml) was added dropwise to a stirred solution of compound 11 (7.00 g, 28 mmol), (S)-(+)-octan-2-ol (3.66 g 28 mmol) and diethyl azodicarboxylate (4.87 g, 28 mmol) in THF (100 ml). The reaction solution was left stirring under nitrogen until completion [reaction monitored by TLC (dichloromethane, silica)]. Upon completion, the solvent was removed in vacuo to yield a colourless solid which was purified by column chromatography (dichloromethane) on silica to yield a colourless oil. Yield 10.01 g (99%), [α]D=−22.4° at 25° C.

WORKUP

后处理

  1. waitThe reaction solution was left
  2. customUpon completion, the solvent was removed in vacuo
  3. customto yield a colourless solid which
  4. customwas purified by column chromatography (dichloromethane) on silica
  5. customto yield a colourless oil
  6. customat 25° C.