Acetic Acid → HCID 22135224, compound

Participants

Reaction Conditions

Reaction Steps

In a 100 ml bomb tube made of stainless steel 10.12 g (30.0 millimoles) of 8-methyl-5-(3-methyl-4-nitro-phenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepine and 50 ml of glacial acetic acid are weighed in. To the suspension at 15–20° C. 5.90 g (90.6 millimoles) of potassium cyanide are added within 5 minutes under cooling with icecold water. The bomb tube is sealed. The reaction mixture is stirred at 70° C. for 24 hours, cooled, stirred with 350 ml of dichloro methane and 350 ml of water and the layers are separated. The aqueous phase is extracted with 150 ml of dichloro methane, the organic phases are washed with 50 ml of water, dried over magnesium sulfate and evaporated. The residue is is crystallized from 100 ml of ether, filtered and washed with ether. Thus 10.40 g of the desired compound are obtained, yield 95%, mp.: 148–151° C.

Provenance & Evidence