反応 #322542

反応方程式

Trifluoroacetic anhydride

Hydrogen peroxide

2,3-bischloromethyl-1,4-dichloro-2-butene

→

2,3-Bischloromethyl-1,4-dichloro-2,3-epoxybutane

溶媒

methylene chloride

methylene chloride

反応条件

後処理

1. 1
   温度chilled in an ice bath
2. 2
   その他was 10° C
3. 3
   温度The reaction mixture was then chilled to 80° C
4. 4
   その他The resulting reaction mixture
5. 5
   温度was warmed to ambient temperature for three hours
6. 6
   温度refluxed for five hours

実験手順

A reaction flask was charged with 145 ml of methylene chloride, chilled in an ice bath, and placed under a positive nitrogen atmosphere. Trifluoroacetic anhydride 51.9 g (0.247 mole) was added in one portion when the pot temperature was 10° C. Hydrogen peroxide solution (50%) 6.9 g (0.101 mole) was then added in several portions. The exotherm raised the pot temperature to 32° C. The reaction mixture was then chilled to 80° C. A solution of 2,3-bischloromethyl-1,4-dichloro-2-butene 5.6 g (25.6 m moles) in methylene chloride 30 ml was added dropwise over a twenty-minute period. The resulting reaction mixture was warmed to ambient temperature for three hours and refluxed for five hours.

出典