HRID1085710

反应详情

EQUATION

反应方程式

HRID 1085710 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of ethyl (RS)-2-[2-(1,1-dimethylethyl)pyrimidin-5-yl]-3,3-dimethylbutanoate (0.07 g), 2,3,5,6-tetrafluoro-4-methylbenzyl alcohol (0.1 g), titanium VI ethoxide (catalytic amount) and dry toluene (2 cm3) was heated at the reflux temperature for 10 hours. After cooling, the solvent was evaporated under reduced pressure to leave a brown gum, which was purified by preparative thin layer chromatography on 20 cm×20 cm×0.2 cm silica gel plates, eluting with dichloromethane containing 2% by volume ethyl acetate, to give the title compound (0.05 g) as an oil which solidified on standing.

WORKUP

后处理

  1. temperaturewas heated at the reflux temperature for 10 hours
  2. temperatureAfter cooling
  3. customthe solvent was evaporated under reduced pressure
  4. customto leave a brown gum, which
  5. customwas purified by preparative thin layer chromatography on 20 cm×20 cm×0.2 cm silica gel plates
  6. washeluting with dichloromethane containing 2% by volume ethyl acetate