反应 #66100

ord-c29a18fee9b8430f971d96da9a294c69

反应方程式

O=C(CBr)C1(Br)CCCC1
2-Bromo-1-(1-bromo-cyclopentyl)-ethanone
Cc1ccccn1
α-picoline
Cc1cccc[n+]1CC(=O)C1=CCCC1.[Br-]
1-(2-Cyclopent-1-enyl-2-oxo-ethyl)-2-methyl-pyridinium bromide salt
收率 117.6%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度at reflux overnight
  2. 2
    温度to cool
  3. 3
    浓缩then concentrated in vacuo
  4. 4
    洗涤The crude mass was washed with 30% ethyl acetate/petroleum ether and diethyl ether

实验过程

2-Bromo-1-(1-bromo-cyclopentyl)-ethanone (3.7 g, 13.7 mmol) and α-picoline (1.02 g, 11.0 mmol) in acetone were heated at reflux overnight. The reaction mixture was allowed to cool then concentrated in vacuo. The crude mass was washed with 30% ethyl acetate/petroleum ether and diethyl ether. 1-(2-Cyclopent-1-enyl-2-oxo-ethyl)-2-methyl-pyridinium bromide salt (3.65 g, 94%) was obtained as a semi-solid material and taken for next step without purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08524705B2uspto-grants-2013_09