Dimethylformamide diethylacetal → Ethyl 3-(N,N-dimethylamino)-2-(1H-imidazol-1-yl)acrylate

HRID 562447노트

반응식

HRID 562447 반응식
[N:1]1([CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH:5]=[CH:4][N:3]=[CH:2]1.C(O[CH:15](OCC)[N:16]([CH3:18])[CH3:17])C>>[CH3:15][N:16]([CH:18]=[C:6]([N:1]1[CH:5]=[CH:4][N:3]=[CH:2]1)[C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH3:17]

참가 물질

3

반응물 2

HCID 70913Dimethylformamide diethylacetalHCID 3798501ethyl 2-(1H-imidazol-1-yl)acetate

생성물 1

HCID 66726242Ethyl 3-(N,N-dimethylamino)-2-(1H-imidazol-1-yl)acrylate

실험 절차

38.0 g (244.9 mmol) of the compound from Example 3A are stirred in 126 ml (108.1 g, 734.7 mmol) of N,N-dimethylformamide diethyl acetal at a bath temperature of 90° C. for 16 h. After cooling, the mixture is concentrated under reduced pressure, the residue is stirred with diisopropyl ether and the solid is filtered off and finally washed with diisopropyl ether. Yield: 49.0 g (95% of theory)

후처리

  1. temperatureAfter cooling
  2. concentrationthe mixture is concentrated under reduced pressure
  3. filtrationthe solid is filtered off
  4. washfinally washed with diisopropyl ether

출처 및 근거

ORD 기록
ord-f25bccf5087346a5946a6563ea7435c9
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08067407B2

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