HRID1242402

反应详情

EQUATION

反应方程式

HRID 1242402 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

0.24 g (1.0 mmol) of the above prepared 2-(5-hydroxy-2-methyl-phenoxy)-2-methyl-propionic acid ethyl ester, 0.31 g (1.10 mmol) of 2-[2-methyl-6-(4-trifluoromethyl-phenyl)-pyridin-3-yl]-ethanol (see below example 70E]) and 0.32 g (1.20 mmol) of triphenylphosphine were dissolved in 10 ml of THF. The stirred reaction mixture was cooled down to 0° C. and a solution of 0.27 g (1.15 mmol) of di-tert.-butyl azodicarboxylate in 5 ml of THF was added drop by drop. Then, the reaction warmed up to ambient temperature. After 20 hours, the solvent was evaporated and the residue purified by chromatography (SiO2, heptane/EtOAc=95:5 to 9:1) to give 0.23 g of the title compound as colorless oil.

WORKUP

后处理

  1. customThe stirred reaction mixture
  2. temperatureThen, the reaction warmed up to ambient temperature
  3. customthe solvent was evaporated
  4. customthe residue purified by chromatography (SiO2, heptane/EtOAc=95:5 to 9:1)