Dimethylformamide dimethyl acetal → 3'-Chloro-3-dimethylamino-2-methylacrylophenone

HRID 231508

反応式

HRID 231508 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:8](=[O:11])[CH2:9][CH3:10])[CH:5]=[CH:6][CH:7]=1.CO[CH:14](OC)[N:15]([CH3:17])[CH3:16]>>[Cl:1][C:2]1[CH:3]=[C:4]([C:8](=[O:11])[C:9]([CH3:10])=[CH:14][N:15]([CH3:16])[CH3:17])[CH:5]=[CH:6][CH:7]=1

参加物

3

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 5871283'-Chloropropiophenone

生成物 1

HCID 544394783'-Chloro-3-dimethylamino-2-methylacrylophenone

実験手順

A mixture of 75.0 g of m-chloropropiophenone and 200 ml of N,N-dimethylformamide dimethyl acetal was stirred and heated at reflux for 16 hours. The mixture was evaporated in vacuo to give a black oil. The oil was subjected to Kugelrohr distillation at 0.5 mm of mercury and the fraction that boils at 110° C. was removed. The residue from the distillation was collected to give 35.0 g of 3'-chloro-3-dimethylamino-2-methylacrylophenone as a black oil.

後処理

  1. temperatureheated
  2. temperatureat reflux for 16 hours
  3. customThe mixture was evaporated in vacuo
  4. customto give a black oil
  5. distillationThe oil was subjected to Kugelrohr distillation at 0.5 mm of mercury
  6. customthe fraction that boils at 110° C. was removed
  7. distillationThe residue from the distillation
  8. customwas collected

出典と根拠

ORDレコード
ord-8d16c1f36b8c45f6b1a124928cf6bdc6
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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