Water → HCID 11176479, compound

Participants

Reaction Steps

1.70 g (5.0 millimoles) of (±)-7,8-dihydro-8-methyl-5-(3-methyl-4-nitro-phenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepine are stirred in 10 ml of acetic anhydride at room temperature for a day. The reaction mixture is poured into a mixture of 100 ml of water and 75 ml of dichloro methane, stirred for an hour and the pH is adjusted to 8 by adding sodium carbonate in portions. The layers are separated, the aqueous phase is extracted twice with 25 ml of dichloro methane each. The united organic phases are washed with 50 ml of saturated sodium chloride solution, dried over magnesium sulfate and evaporated. The crude product obtained is recrystallized from 15 ml of ethanol. Thus 1.65 g of the desired product are obtained, yield 87%, mp.: 178–181° C.

Provenance & Evidence