HRID1780063

反应详情

EQUATION

反应方程式

HRID 1780063 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.6 ml (3.8 mmol) of diethyl azodicarboxylate is added dropwise at 0° C. to 1.00 g (3.80 mmol) of triphenylphosphine in 15 ml of tetrahydrofuran, and the mixture is stirred at room temperature for 30 minutes. 0.78 g (2.5 mmol) of 3-chloro-5-hydroxy-2-(4-octyloxyphenyl)-pyridine and 0.6 ml (3.8 mmol) of 1-octanol are subsequently added. After a reaction time of 18 hours at room temperature, the solvent is removed by distillation and the residue is purified by chromatography (silica gel, dichloromethane). Recrystallization from acetonitrile gives 0.63 g of 3-chloro-5-octyloxy-2-(4-octyloxyphenyl)pyridine. ##STR19## The compound has the phase sequence: X 32.2 (6.5) N 17 I.

WORKUP

后处理

  1. customAfter a reaction time of 18 hours at room temperature, the solvent is removed by distillation
  2. customthe residue is purified by chromatography (silica gel, dichloromethane)
  3. customRecrystallization from acetonitrile