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

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Reaction Steps

5 ml of sulfuryl chloride in 100 ml methylene chloride are added dropwise to a solution of 12 g of 4-chloroacetyl-9,10-dihydro-4H-thieno[3,4-b][1,5]benzodiazepin-10-one in 300 ml of methylene chloride at 20° C. The mixture is left to stand at room temperature for a further 12 hours and is then extracted by shaking it with sodium bicarbonate solution and washing it with water; the organic phase is dried and concentrated. The residue is made to crystallize with a little methanol. 7 g of 3-chloro-4-chloroacetyl-9,10-dihydro-4H-thieno[3,4-b][1,5]benzodiazepin-10-one is thus obtained, m. 214° to 216° C. (acetonitrile).

Provenance & Evidence