HRID652038

反应详情

EQUATION

反应方程式

HRID 652038 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 14 g. of tert-butyl ethyl malonate in 5 ml. of 1,2-dimethoxyethane is added to a suspension of 2.0 g. of sodium hydride in 1,2-dimethoxyethane under argon. A solution of 8.4 g. of 4-[14-(trimethylsilyl)tetradecylamino]benzoyl chloride hydrochloride in 1,2-dimethoxyethane is then added. The reaction mixture is refluxed for 5 hours, cooled, poured on ice and extracted with ether. The ether solution is washed with water and saturated sodium chloride solution, dried with anhydrous sodium sulfate and evaporated to dryness. The residue is then recrystallized to yield the title compound.

WORKUP

后处理

  1. temperatureThe reaction mixture is refluxed for 5 hours
  2. temperaturecooled
  3. additionpoured on ice
  4. extractionextracted with ether
  5. washThe ether solution is washed with water and saturated sodium chloride solution
  6. dry with materialdried with anhydrous sodium sulfate
  7. customevaporated to dryness
  8. customThe residue is then recrystallized