Glycine ethyl ester → HCID 73680293, 화합물

HRID 1981044노트

반응식

HRID 1981044 반응식
[Cl:1][C:2]1[CH:15]=[CH:14][C:5]([O:6][C:7](=[CH:10][N:11]([CH3:13])C)[CH:8]=[O:9])=[CH:4][CH:3]=1.NC[C:18]([O:20][CH2:21][CH3:22])=[O:19].[OH-].[Na+]>C(O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:6][C:7](=[CH:10][NH:11][CH2:13][C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH:8]=[O:9])=[CH:14][CH:15]=1

참가 물질

5

반응물 3

HCID 12176Glycine ethyl esterHCID 14798Sodium HydroxideHCID 54237126HCID 54237126, 화합물

생성물 1

HCID 73680293HCID 73680293, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2-(4-Chlorophenoxy)-3-dimethylaminoacrylaldehyde (11.3 g., 50 mmoles) was dissolved in 200 ml. of ethanol, mixed with a solution of ethyl glycinate (14 g., 100 mmoles) in 90 ml. of 1N sodium hydroxide and refluxed for 15 hours. Ethanol was evaporated in vacuo, the aqueous residue diluted with 150 ml. of water and product extracted into 200 ml. of ethyl acetate. The ethyl acetate was back-washed with water and concentrated to an oil. Trituration of the oil with 100 ml. of ether gave crystalline 2-(4-chlorophenoxy)-3-carbethoxymethylaminoacrylaldehyde in two crops (7.3 g., Rf 0.55 on silica gel thin layer chromatography with ethyl acetate-1/hexane-1/5% acetic acid as eluant).

후처리

  1. customEthanol was evaporated in vacuo
  2. additionthe aqueous residue diluted with 150 ml
  3. extractionof water and product extracted into 200 ml
  4. washThe ethyl acetate was back-washed with water
  5. concentrationconcentrated to an oil

출처 및 근거

ORD 기록
ord-4b2a7dcf62af4c47973c6eb50dcc0e42
출처 데이터셋
uspto-grants-1985_04
특허 번호
US04511576

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