Chloroacetyl chloride → 4-chloroacetyl-9,10-dihydro-4H-thieno[3,4-b][1,5]benzodiazepin-10-one

Participants

Reaction Steps

2.2 g of chloroacetyl chloride and 2 ml of triethylamine are simultaneously added dropwise to a boiling solution of 2.2 g of 9,10-dihydro-4H-thieno[3,4-b][1,5]benzodiazepin-10-one in 30 ml of absolute dioxane in the course of 40 minutes, and the mixture is stirred for a further 3 hours. It is then allowed to cool and is filtered; the filtrate is concentrated to dryness; the residue is chromatographed over a silica gel column by means of a mixture of petroleum ether/ethyl acetate (1:1), and the product is recrystallized from toluene to yield 2.0 g of 4-chloroacetyl-9,10-dihydro-4H-thieno[3,4-b][1,5]benzodiazepin-10-one (m. 220° C.).

Provenance & Evidence