Water → HCID 22135219, compound

Participants

Reaction Steps

To a solution of 3.40 g (20.0 millimoles) of silver(I)nitrate and 25 ml of water a solution of 1.60 g (4.0 millimoles) of sodium hydroxide and 25 ml of water is added. The mixture is stirred for 10 minutes, diluted with 50 ml of tetrahydrofurane and 3.51 g (10.0 millimoles) of 8-formyl-5-(3-methyl-4-nitro-phenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepine are added under cooling with icecold water. The reaction mixture is stirred at room temperature for 5 hours, filtered on a coal-bed and washed with cold water. The pH of the solution is adjusted to 2 with 6 N hydrochloric acid. After cooling the precipitated product is filtered and washed with 10 ml of cold water. Thus 2.61 g of the desired compound are obtained, yield 71%, mp.: 185–186° C.

Provenance & Evidence