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

HRID 231530

反応式

HRID 231530 の反応式
[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]

参加物

3

反応物 2

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

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bb1052c824674d639b76eec8fbf3e767
出典データセット
uspto-grants-1989_07
特許番号
US04847256

関連ノート

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