Acetophenone → 2-Chloro-3-phenylprop-2-enal

HRID 444300ノート

反応式

HRID 444300 の反応式
P(Cl)(Cl)([Cl:3])=O.[C:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=O)[CH3:7].[C:15]([O-:18])(=O)C.[Na+]>CN(C)C=O.O>[Cl:3][C:7](=[CH:6][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH:15]=[O:18]

参加物

6

反応物 3

HCID 7410AcetophenoneHCID 24813Phosphorus oxychloride2 回HCID 517045Sodium Acetate

生成物 1

HCID 290422-Chloro-3-phenylprop-2-enal

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
0 °C

実験手順

β chlorocinnamaldehyde was prepared by the following method. Phosphoryl chloride (24 ml, 0.26 mol.) was slowly added to anhydrous dimethyl formamide (40 ml) maintaining a temperature of 0° C. and the resulting solution stirred for 30 minutes. Acetophenone (24 g 0.2 mol.) was also dissolved in anhydrous dimethyl formamide (25 ml) and the mixture slowly added to the phosphoryl chloride solution. Whilst stirring, the reaction mixture was allowed to attain room temperature, stirred for two hours and then poured into an agitated solution of sodium acetate (300 g) in water (750 ml), After stirring for 30 minutes the product was extracted into ether, the ether extracts were dried over magnesium sulphate and the ether was then removed to yield 28.8 g of crude product which was used without further purification as follows.

後処理

  1. stirringWhilst stirring
  2. customto attain room temperature
  3. stirringstirred for two hours
  4. stirringAfter stirring for 30 minutes the product
  5. extractionwas extracted into ether
  6. dry with materialthe ether extracts were dried over magnesium sulphate
  7. customthe ether was then removed

出典と根拠

ORDレコード
ord-34e0e119e042404f9d996d760c9d86d1
出典データセット
uspto-grants-1981_04
特許番号
US04263394

反応ノート

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