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8-BROMO-2-CHLORO-11-ETHYL-5-METHYL-5H-DIPYRIDO[3,2-B:2',3'-E][1,4]DIAZEPIN-6(11H)-ONE synthesis

7synthesis methods
6H-Dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one, 8-bromo-2-chloro-11-ethyl-5,11-dihydro-

189393-15-5
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8-BROMO-2-CHLORO-11-ETHYL-5-METHYL-5H-DIPYRIDO[3,2-B:2',3'-E][1,4]DIAZEPIN-6(11H)-ONE

189393-17-7
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Yield:189393-17-7 94%

Reaction Conditions:

with NaH in N,N-dimethyl-formamide;

Steps:

II.e e

e 8-Bromo-2-chloro-5,11-dihydro-11-ethyl-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one Solid NaH (60% oil dispersion, 3.46 g, 86.1 mmol) was added over 30 min to a solution of 8-bromo-2-chloro-5,11-dihydro-11-ethyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (23.4 g, 66.3 mmol) in DMF (220 mL) at 50° C. The mixture was stirred at 50° C. for 1 h then was allow to cool to room temperature. The mixture was poured into water (1 L) and the resulting suspension was filtered. The solid was successively washed with water and hexane then dried under reduced pressure to give the title compound (23.0 g, 94% yield).

References:

US2002/28807,2002,A1

8-BROMO-2-CHLORO-11-ETHYL-5-METHYL-5H-DIPYRIDO[3,2-B:2',3'-E][1,4]DIAZEPIN-6(11H)-ONE Related Search: