Hydrogen Peroxide → HCID 57295667, compound

Temperature

32 °C

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.

1. temperaturechilled in an ice bath
2. customwas 10° C
3. temperatureThe reaction mixture was then chilled to 80° C
4. customThe resulting reaction mixture
5. temperaturewas warmed to ambient temperature for three hours
6. temperaturerefluxed for five hours

ORD record

ord-8af3843fb05f4032813e5f6daddadaa2

Source dataset

uspto-grants-1997_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05597978