반응 #945

ord-968da5d345074707bd8ae7f036b4987e

반응 방정식

O=Cc1ccccc1
benzaldehyde
CCOC(=O)C(N)CC.Cl
product
CCOC(=O)C(N)CC.Cl
Ethyl 2-aminobutyrate hydrochloride
O=S(=O)([O-])[O-].[Mg+2]
magnesium sulphate
CCN(CC)CC
triethylamine
CCOC(=O)C(CC)N=Cc1ccccc1
desired product
수율 88.9%
CCOC(=O)C(CC)N=Cc1ccccc1
Ethyl 2-benzylideneaminobutyrate
수율 88.9%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과then filtered
  2. 2
    농축The filtrate was concentrated
  3. 3
    기타triturated in diethyl ether
  4. 4
    여과filtered
  5. 5
    농축concentrated

실험 절차

A solution of the product from step (a) (149.6 g), magnesium sulphate (74.3 g), and triethylamine (246 ml) in dichloromethane (1500 ml) was stirred at room temperature under nitrogen and benzaldehyde (94.9 g, Aldrich) was added dropwise. The mixture was stirred at room temperature for 3 hours then filtered. The filtrate was concentrated, triturated in diethyl ether, filtered and concentrated to yield the desired product as a yellow oil (174 g). 1H NMR consistent with the proposed structure.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05723458uspto-grants-1998_03