反应详情

2.0 g of 4-chloroacetyl-9,10-dihydro-4H-thieno[3,4-b][1,5]benzodiazepin-10-one, 6 ml of 40% strength aqueous dimethylamine solution and 10 ml of methylene chloride are stirred at 35° C. for 2 hours; 0.35 g of sodium carbonate is added, and the mixture is concentrated to dryness in vacuo. A little water is added; the solution is extracted repeatedly by shaking it with chloroform, and the organic solution is dried with sodium sulfate and concentrated to dryness. 1.9 g of 4-(dimethylaminoacetyl)-9,10-dihydro-4H-thieno[3,4-b][1,5]benzodiazepin-10-one are thus obtained. 4-(Diethylaminoacetyl)-9,10-dihydro-3-methyl-4H-thieno[3,4-b][1,5]benzodiazepin-10-one [m. 196°-197° C. (from toluene)] is obtained analogously by reacting 4-chloroacetyl-9,10-dihydro-3-methyl-4H-thieno[3,4-b][1,5]benzodiazepin-10-one with a corresponding amount of diethylamine (instead of dimethylamine).

1. concentrationthe mixture is concentrated to dryness in vacuo
2. additionA little water is added
3. extractionthe solution is extracted repeatedly
4. dry with materialthe organic solution is dried with sodium sulfate
5. concentrationconcentrated to dryness