4'-Chloropropiophenone → 4'-Chloro-3-dimethylamino-2-methylacrylophenone

HRID 231509

반응식

HRID 231509 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:11])[CH2:9][CH3:10])=[CH:4][CH:3]=1.CO[CH:14](OC)[N:15]([CH3:17])[CH3:16]>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8](=[O:11])[C:9]([CH3:10])=[CH:14][N:15]([CH3:16])[CH3:17])=[CH:6][CH:7]=1

참가 물질

3

반응물 2

HCID 226974'-ChloropropiophenoneHCID 78373Dimethylformamide dimethyl acetal

생성물 1

HCID 538154144'-Chloro-3-dimethylamino-2-methylacrylophenone

실험 절차

A mixture of 50.0 g of p-chloropropiophenone and 200 ml of N,N-dimethylformamide dimethyl acetal was stirred and heated at reflux for 28 hours. The reaction mixture was evaporated in vacuo to give a yellow oil. The oil was then subjected to Kugelrohr distillation. The residual oil from the distillation was collected and triturated with hexane to provide crystals. The solid was collected by filtration and gave 21.5 g of 4'-chloro-3-dimethylamino-2-methylacrylophenone as yellow crystals, mp 45°-47° C.

후처리

  1. temperatureheated
  2. temperatureat reflux for 28 hours
  3. customThe reaction mixture was evaporated in vacuo
  4. customto give a yellow oil
  5. distillationThe oil was then subjected to Kugelrohr distillation
  6. distillationThe residual oil from the distillation
  7. customwas collected
  8. customtriturated with hexane
  9. customto provide crystals
  10. filtrationThe solid was collected by filtration

출처 및 근거

ORD 기록
ord-f46b79335d2345a3a60be1bf6ca49e28
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04847256

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