Hydrogen Peroxide → 2,6-Dichloronitrosobenzene

Temperature

5 °C

To a solution of 2,6-dichloroaniline (42.3 g, 0.26 mole) in glacial acetic acid (520 ml) in a 1 litre conical flask at room temperature, was added 100 vol hydrogen peroxide (157 ml, 1.38 mole). The flask was plugged with absorbant cotton, and set aside on a thermostatically controlled water bath at a temperature of 25°-30° C. for 70 hours. The flask was then cooled to 5° C., and the crystalline solid collected on a sintered glass funnel, washed with ethanol-pet. ether (40°-60°) (200 ml, 1:1, v/v), and dried in an oven at 90° C. The buff leaflets weighed 40.25 g (87.6%) m.p. 171°-172° C.

1. customthe crystalline solid collected on a sintered glass funnel
2. washwashed with ethanol-pet. ether (40°-60°) (200 ml, 1:1
3. customv/v), and dried in an oven at 90° C

ORD record

ord-1fc1d461fe544ebbaad5c966eed74fd6

Source dataset

uspto-grants-1982_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04358595