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

HRID 231509

反応式

HRID 231509 の反応式
[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

参加物

3

反応物 2

HCID 226974'-ChloropropiophenoneHCID 78373Dimethylformamide dimethyl acetal

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f46b79335d2345a3a60be1bf6ca49e28
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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