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

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Reaction Steps

10.4 ml of chloroacetyl chloride are added dropwise at room temperature to a suspension of 18.8 g of 9,10-dihydro-4H-thieno[3,4-b][1,5]benzodiazepin-10-one in 500 ml of dioxane, whereupon a clear solution is formed. The solution is left to stand for 3 hours and is then concentrated to dryness; the obtained 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 thus-dried solution yields 4-chloroacetyl-9,10-dihydro-4H-thieno[3,4-b][1,5]benzodiazepin-10-one (m. 220° C.).

Provenance & Evidence