反应 #945

ord-968da5d345074707bd8ae7f036b4987e

反应方程式

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
收率 88.9%
CCOC(=O)C(CC)N=Cc1ccccc1
Ethyl 2-benzylideneaminobutyrate
收率 88.9%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤then filtered
  2. 2
    浓缩The filtrate was concentrated
  3. 3
    其他triturated in diethyl ether
  4. 4
    过滤filtered
  5. 5
    浓缩concentrated

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05723458uspto-grants-1998_03