反应详情

A mixture of 11-(chloroacetyl)-5,11-dihydro-6H-pyrido-[2,3-b][1,4]benzodiazepin-6-one (97.6 g, 0.339 mol), 2-[(diethylamino)methyl]piperidine (64.0 g, 0.376 mol), sodium carbonate (36.0 g, 0.34 mol) and n-propanol (1.7 liters) is refluxed for 5 hours. The reaction mixture is filtered while hot then left to stand for 12 hours at ambient temperature, after which the desired product is found to have precipitated in crystalline form. The substance is suction filtered, washed 3 times, each time with n-propanol (100 ml), and dried in a vacuum drying chamber. Colorless crystals (119.5 g) are obtained, Mp. 226°-229° C.

1. temperatureis refluxed for 5 hours
2. filtrationThe reaction mixture is filtered while hot
3. waitthen left
4. customto have precipitated in crystalline form
5. filtrationfiltered
6. washwashed 3 times
7. dry with materialeach time with n-propanol (100 ml), and dried in a vacuum
8. customdrying chamber