反应详情

To a mixture of 2-chloro-5,11-dihydro-11-ethyl-8-[trans-2-(4-pyridyl)ethen-1-yl]-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (2.3 g, 5.9 mmol) and palladium black (0.25 g) in 30 mL of 1,4-dioxane was added a solution of sodium hypophosphite (0.82 g 7.7 mmol) in 15 mL of water. The reaction mixture was heated at 80°-90° C. for 3 hours. The reaction mixture was then filtered through Celite and extracted with ethyl acetate. The product was purified by chromatography over silica gel, eluting with methanol/dichloromethane, and recrystallized from ethyl acetate/hexanes to give 1.75 g of the title compound as colorless crystals, m.p. 158°-159° C.

1. temperatureThe reaction mixture was heated at 80°-90° C. for 3 hours
2. filtrationThe reaction mixture was then filtered through Celite
3. extractionextracted with ethyl acetate
4. customThe product was purified by chromatography over silica gel
5. washeluting with methanol/dichloromethane
6. customrecrystallized from ethyl acetate/hexanes