Benzaldehyde → Ethyl 2-benzylideneaminobutyrate

HRID 398809

反応式

HRID 398809 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) (149.6 g), magnesium sulphate (74.3 g), and triethylamine (246 ml) in dichioromethane (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.

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-3c5cb32813c44d02b95d64edcf9341ec
出典データセット
uspto-grants-1998_10
特許番号
US05817652

関連ノート

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