반응 #1095846

ord-79c785bba81c462a9ad6d462521a90f8

반응 방정식

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

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타After 19 h the solution was partitioned with dichloromethane (3×100 mL)
  2. 2
    건조The organic layer was dried with anhydrous sodium sulfate
  3. 3
    여과filtered
  4. 4
    기타evaporated
  5. 5
    workup.DISTILLATIONThe residue was distilled
  6. 6
    기타to afford AA (28.8 g, 61%)

실험 절차

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07973020B2uspto-grants-2011_07