Benzaldehyde → Ethyl 2-benzylideneaminobutyrate

HRID 849

반응식

HRID 849 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 10331026Ethyl 2-benzylideneaminobutyrate수율 88.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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.

후처리

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

출처 및 근거

ORD 기록
ord-968da5d345074707bd8ae7f036b4987e
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05723458

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