HRID1601445

反应详情

EQUATION

反应方程式

HRID 1601445 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine t-butyl 1-piperazinecarboxylate (10.47 g, 56.2 mmol), ethyl acrylate (8 mL) in ethanol (30 mL). Heat at reflux. After 5.5 hours, cool the reaction mixture and evaporate in vacuo to give a residue. Combine the residue and diethyl ether (200 mL) and extract with a 1M aqueous solution of hydrochloric acid. Adjust the pH of the aqueous layer to basic using sodium bicarbonate and then extract with ethyl acetate. Dry the organic layer over MgSO4, filter, and evaporate in vacuo to give t-butyl 4-carboethoxyethyl-1-piperazinecarboxylate.

WORKUP

后处理

  1. temperatureHeat
  2. temperatureat reflux
  3. temperaturecool the reaction mixture
  4. customevaporate in vacuo
  5. customto give a residue
  6. extractionextract with a 1M aqueous solution of hydrochloric acid
  7. extractionextract with ethyl acetate
  8. dry with materialDry the organic layer over MgSO4
  9. filtrationfilter
  10. customevaporate in vacuo