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

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Reaction Steps

8 g of 9,10-dihydro-3-methyl-4H-thieno[3,4-b][1,5]benzodiazepin-10-one and 5.6 ml of chloroacetyl chloride are boiled in 160 ml of dioxane (containing 8 g of ground potassium carbonate) under reflux for 8 hours. The thus-obtained suspension is concentrated to dryness; the resulting residue is taken up in toluene; the toluene mixture is washed with sodium bicarbonate solution and then with water, and the toluene solution is dried over sodium sulfate. Concentration of the dried toluene solution yields 4-chloroacetyl-9,10-dihydro-3-methyl-4H-thieno[3,4-b][1,5]benzodiazepin-10-one (m. 156° to 158° C.).

Provenance & Evidence