反应 #1095846

ord-79c785bba81c462a9ad6d462521a90f8

反应方程式

C=CC(=O)OCC
ethyl acrylate
CCOC(=O)CN.Cl
ethyl glycinate hydrochloride
[Na+].[OH-]
sodium hydroxide
CCOC(=O)CCNCC(=O)OCC
Diethyl-2-azabutane-1,4-dicarboxylate

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他After 19 h the solution was partitioned with dichloromethane (3×100 mL)
  2. 2
    干燥The organic layer was dried with anhydrous sodium sulfate
  3. 3
    过滤filtered
  4. 4
    其他evaporated
  5. 5
    workup.DISTILLATIONThe residue was distilled
  6. 6
    其他to afford AA (28.8 g, 61%)

实验过程

A 4.7 M aqueous solution of sodium hydroxide (50 mL) was added into a stirred, ice-cooled solution of ethyl glycinate hydrochloride (32.19 g, 0.23 mole) in water (50 mL). Then, ethyl acrylate (23.1 g, 0.23 mole) was added and the mixture was stirred at room temperature until completion of the reaction was ascertained by TLC. After 19 h the solution was partitioned with dichloromethane (3×100 mL). The organic layer was dried with anhydrous sodium sulfate, filtered and evaporated. The residue was distilled to afford AA (28.8 g, 61%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07973020B2uspto-grants-2011_07