Water → HCID 135848416, compound

Participants

Reaction Steps

15.7 g (0.055 mol) of 1,3-dihydro-5-(o-nitrophenyl)-2H-thieno[2,3-e]-1,4-diazepin-2-one are warmed to 60° C. in 40 ml of absolute pyridine and there are added with vigorous stirring 15.7 g of finely powdered phosphorus pentasulphide. The mixture is stirred for a further 1.5 hours at this temperature, subsequently poured on to 500 g of ice and 500 ml of water with vigorous stirring and stirred for 2 hours. The resulting precipitate is filtered under a vacuum and washed with a large amount of water. The precipitate is suspended in water and shaken out thoroughly with 500 ml of methylene chloride each time. After drying, the organic phase is evaporated under reduced pressure and the residue refluxed with a small amount of chloroform. After completion of the crystallization in a refrigerator, there is obtained 1,3-dihydro-5-(o-nitrophenyl)-2H-thieno[2,3-e]-1,4-diazepine-2-thione which, after recrystallization from absolute methanol, melts at 207°-209° C.

Provenance & Evidence