Glycine ethyl ester → HCID 73680293, 화합물

HRID 894089노트

반응식

HRID 894089 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 1 N 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 this 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-a5d5950fa3c04e47af49fc7d0bff273e
출처 데이터셋
uspto-grants-1981_08
특허 번호
US04282242

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