Ethanone, 1-(3,4-dichlorophenyl)- → 1-(3,4-Dichlorophenyl)-3-(dimethylamino)prop-2-en-1-one

HRID 231530

반응식

HRID 231530 반응식
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([Cl:10])=[C:6]([Cl:11])[CH:5]=1)=[O:3].CO[CH:14](OC)[N:15]([CH3:17])[CH3:16]>>[Cl:11][C:6]1[CH:5]=[C:4]([C:2](=[O:3])[CH:1]=[CH:14][N:15]([CH3:17])[CH3:16])[CH:9]=[CH:8][C:7]=1[Cl:10]

참가 물질

3

반응물 2

HCID 75841Ethanone, 1-(3,4-dichlorophenyl)-HCID 78373Dimethylformamide dimethyl acetal

생성물 1

HCID 28051561-(3,4-Dichlorophenyl)-3-(dimethylamino)prop-2-en-1-one

실험 절차

A mixture of 50.0 g of 3,4-dichloroacetophenone and 75 ml of N,N-dimethylformamide dimethyl acetal was heated under reflux for 6 hours, then allowed to cool for 16 hours. The crystalline precipitate was collected by filtration, washed with hexane and dried. The addition of hexane to the above filtrate precipitated some additional product which was collected by filtration. The precipitates were combined, washed with hexane and dried in vacuo to give 55.0 g of 3',4'-dichloro-3-dimethylaminoacrylophenone as bright yellow crystals.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 6 hours
  3. temperatureto cool for 16 hours
  4. filtrationThe crystalline precipitate was collected by filtration
  5. washwashed with hexane
  6. customdried
  7. additionThe addition of hexane to the above filtrate
  8. customprecipitated some additional product which
  9. filtrationwas collected by filtration
  10. washwashed with hexane
  11. customdried in vacuo

출처 및 근거

ORD 기록
ord-bb1052c824674d639b76eec8fbf3e767
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04847256

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