反応 #1121718

ord-ebb2d69525ac483c93f0a1552252adff

反応方程式

CC(=O)c1ccccc1
acetophenone
CC(C)(C)c1ccc(C(=O)Cl)cc1
4-tert-butylbenzoyl chloride
C=C(OC(=O)c1ccc(C(C)(C)C)cc1)c1ccccc1
1-phenylvinyl 4-tert-butylbenzoate
収率 57.0%

溶媒

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.WAITThe mixture was then left
  2. 2
    温度to cool
  3. 3
    抽出extracted with dichloromethane
  4. 4
    乾燥The organic phase was dried over magnesium sulfate
  5. 5
    その他the solvent was removed under reduced pressure
  6. 6
    その他A 2.12 g sample was purified by flash chromatography (hexane:dichloromethane 3:1)

実験手順

A mixture of 4.16 g (21.62 mmol) of acetophenone trimethylsilylenol, 4.33 g (22.01 mmol) of 4-tert-butylbenzoyl chloride and 136 mg of mercuric chloride was heated at 100° C. for 2 h. The mixture was then left to cool, water was added over the reaction crude and extracted with dichloromethane. The organic phase was dried over magnesium sulfate and the solvent was removed under reduced pressure. A 2.12 g sample was purified by flash chromatography (hexane:dichloromethane 3:1) giving 1.17 g of 1-phenylvinyl 4-tert-butylbenzoate. Yield 57%.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08545816B2uspto-grants-2013_10