반응 #322542

반응 방정식

Trifluoroacetic anhydride

Hydrogen peroxide

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

→

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

용매

methylene chloride

methylene chloride

반응 조건

후처리

1. 1
   온도chilled in an ice bath
2. 2
   기타was 10° C
3. 3
   온도The reaction mixture was then chilled to 80° C
4. 4
   기타The resulting reaction mixture
5. 5
   온도was warmed to ambient temperature for three hours
6. 6
   온도refluxed for five hours

실험 절차

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.

출처