تفاعل #4264

معادلة التفاعل

propargylamine

11-chlorocarbonyl-5,11-dihydro-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one

triethylamine

→

5,11-Dihydro-11-[[(2-propynyl)-amino]carbonyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one

المذيبات

chloroform

ظروف التفاعل

المعالجة

1. 1
   أخرىrises to 35° C
2. 2
   ترشيحfiltered over activated charcoal
3. 3
   أخرىthe reaction solution is evaporated to dryness in vacuo
4. 4
   أخرىis obtained in the form of a colourless crystalline mass in a yield of 20.7 g (71% of theory)

الإجراء التجريبي

5.5 g (0.1 mol) of propargylamine were added dropwise with stirring at ambient temperature to a suspension of 27.3 g (0.1 mol) of 11-chlorocarbonyl-5,11-dihydro-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one and 10.0 g (0.1 mol) of triethylamine in 500 ml of chloroform, whereupon the temperature rises to 35° C. The mixture is stirred for a further 30 minutes at 40° C., then filtered over activated charcoal and the reaction solution is evaporated to dryness in vacuo. After the oily residue has been decocted with ethyl acetate the desired product is obtained in the form of a colourless crystalline mass in a yield of 20.7 g (71% of theory).

المصدر