反应详情

A solution of 2-chloro-5,11-dihydro-11-ethyl-8-[2-(4-pyridyl)ethyl]-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (78 mg, 0.2 mmol), Sodium cyanide impregnated alumina (2 g/4 g, 0.44 g, 4.5 mmol), and tetrakis(triphenylphosphine)palladium(0) (45 mg, 0.04 mmol) in 5 mL of toluene was heated at 100° C. under argon for 8 hours. The reaction mixture was filtered, and the collected solid was washed with ethyl acetate. The filtrate was concentrated to give a yellow oil, which was purified by flash chromatography (elution with isopropannol-hexanes) and recrystallization (ethyl acetate-hexanes) to afford 11.5 mg (15%) of the title compound, m.p. 149°-150° C.

1. filtrationThe reaction mixture was filtered
2. washthe collected solid was washed with ethyl acetate
3. concentrationThe filtrate was concentrated
4. customto give a yellow oil, which
5. customwas purified by flash chromatography (elution with isopropannol-hexanes) and recrystallization (ethyl acetate-hexanes)