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10189-78-3

6,11-DIHYDRO-5H-PYRIDO[2,3-B][1,5]BENZODIAZEPIN-5-ONE synthesis

3synthesis methods
-

Yield:10189-78-3 98.9 g (83%)

Reaction Conditions:

in dichloromethane;cyclohexanol;

Steps:

23.A Step A.

Step A. 6,11-Dihydro-5H-pyrido[2,3-b][1,5]benzodiazepin-5-one 1:1 salt with hydrochloric acid A mixture of 1,2-phenylene diamine (52 g, 480 mmol) and chloro nicotinic acid (76 g, 482 mmol) in cyclohexanol (480 mL) was refluxed under nitrogen for 2.5 hours. A precipitate appeared soon after the heating was initiated. The warm reaction mixture was carefully poured onto ice-cold dichloromethane (1000 mL) under vigorous stirring. The semisolid mass was collected, washed thoroughly with dichloromethane and dried in vacuo to yield 98.9 g (83%) of the title compound which was used in the next step without further purification.

References:

US5932745,1999,A