1,1-Dichloroethane → HCID 20516775, compound

Participants

Reaction Steps

5 g (14.25 mmol) of 7-amino-6,8-dichloro-5-(o-fluorophenyl)-1,3-dihydro-1-methyl-2H-1,4-benzodiazepin-2-one are dissolved in 325 ml of 1,2-dichloroethane under reflux. The still hot solution is subsequently added dropwise while stirring and cooling with ice to 3.73 g (37.65 mmol) of phosgene in 50 ml of ice-cold 1,2-dichloroethane, the addition being carried out in such a manner that the temperature of the mixture does not exceed 20° C. The mixture is heated under reflux for 1 hour, 80 ml of dichloroethane are allowed to distill off and 80 ml of fresh dichloroethane are added thereto. While cooling with ice, argon is conducted directly into the solution until it has reached a temperature of 10° C. There is thus obtained a 1,2-dichloroethane solution of [6,8-dichloro-5-(o-fluorophenyl)-2,3-dihydro-1-methyl-2-oxo-1H-1,4-benzodiazepin-7-yl]isocyanate.

Provenance & Evidence