Potassium Carbonate → HCID 22135226, compound

Participants

Reaction Steps

2.03 g (25.0 millimoles) of methoxy-amine hydro-chloride and 3.45 g (25.0 millimoles) of potassium carbonate are stirred in 75 ml of anhydrous dimethyl formamide for half an hour whereupon 2.17 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-7-carboxylic acid-imidazolide are added. The reaction mixture is stirred for 16 hours, whereupon the solvent is evaporated at a pressure of 55 Pa. The residue is suspended in 100 ml of water, stirred for half an hour, washed with 50 ml of water and dried. The crude product is recrystallized from 30 ml of acetonitrile and washed with 10 ml of diethyl ether. Thus 1.59 g of the desired compound are obtained, yield 77%, mp.: 192–195° C.

Provenance & Evidence