HRID75104

反应详情

EQUATION

反应方程式

HRID 75104 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1.210 g (5.99 mmol) of diisopropyl azodicarboxylate is added dropwise to a solution, cooled to 0° C., under an argon atmosphere, of 0.974 g (4.99 mmol) of 3′-hydroxybiphenyl-3-carbonitrile, 1.205 g (5.99 mmol) of tert-butyl 4-hydroxypiperidine-1-carboxylate and 1.570 g (5.99 mmol) of triphenylphosphine in 12 ml of tetrahydrofuran. The mixture is subsequently stirred at ambient temperature overnight. 15 g of silica are added and the mixture is evaporated to dryness. The product is purified by chromatography on silica gel, elution being carried out with a 10:90 and then 15:85 mixture of ethyl acetate and cyclohexane, in order to obtain 1.538 g (4.06 mmol) of product in the form of a colourless oil.

WORKUP

后处理

  1. addition15 g of silica are added
  2. customthe mixture is evaporated to dryness
  3. customThe product is purified by chromatography on silica gel, elution
  4. addition15:85 mixture of ethyl acetate and cyclohexane