Benzaldehyde → Ethyl 2-benzylideneaminobutyrate

HRID 1376401

反応式

HRID 1376401 の反応式
Cl.[NH2:2][CH:3]([CH2:9][CH3:10])[C:4]([O:6][CH2:7][CH3:8])=[O:5].S([O-])([O-])(=O)=O.[Mg+2].C(N(CC)CC)C.[CH:24](=O)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>ClCCl>[CH:24](=[N:2][CH:3]([CH2:9][CH3:10])[C:4]([O:6][CH2:7][CH3:8])=[O:5])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1

参加物

6

反応物 4

HCID 240BenzaldehydeHCID 8471TriethylamineHCID 24083Sulfuric acid magnesium salt (1:1)HCID 12844023Ethyl 2-Aminobutyrate Hydrochloride

生成物 1

HCID 10331026Ethyl 2-benzylideneaminobutyrate収率 88.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of the product from step (a) (149.57 g), magnesium sulphate (74.32 g), and triethylamine (246 ml) in dichloromethane (1500 ml) was stirred at room temperature under nitrogen and benzaldehyde (94.91 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 consistent with the proposed structure.

後処理

  1. filtrationthen filtered
  2. concentrationThe filtrate was concentrated
  3. customtriturated in diethyl ether
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-381ba95342884d3da1f29250b2753f2c
出典データセット
uspto-grants-1997_09
特許番号
US05663165

関連ノート

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