反应 #1121718

ord-ebb2d69525ac483c93f0a1552252adff

反应方程式

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
收率 57.0%

溶剂

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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%.

来源

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