Water → HCID 86760093, compound

Participants

Reaction Steps

1.76 g (5.0 millimoles) of 5-(3-methyl-4-nitro-phenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepine-8-carboxylic acid-amide are suspended in a mixture of 75 ml ethanol and 75 ml of dichloro methane, whereupon 0.19 g (5.0 millimoles) of sodium-[tetrahydrido-borate(IV)] are added in one portion and a solution of 0.55 g (5.0 millimoles) of calcium chloride in 25 ml of ethanol is added dropwise. The reaction mixture is stirred at room temperature for 25 hours and evaporated in vacuo. The residue is heated to boiling in 100 ml of water for half an hour and filtered hot. The crude product obtained is heated to boiling in 50 ml of acetonitrile for half an hour, cooled with icecold water, filtered and washed with 20 ml of diethyl ether. Thus 1.27 g of the desired compound are obtained, yield 69%, mp.: 246–249° C.

Provenance & Evidence