反应详情

温度

125 °C

A mixture containing 5,11-dihydro-11-ethyl-8-iodo-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]-diazepin-6-one (0.7 g, 1.9 mmol), 4-vinylpyridine (0.3 mL, 2.9 mmol), bis(triphenylphosphine)palladium(II) chloride (60 mg, 0.09 mmol), triethylamine (1.8 mL, 12.8 mmol), and 1 crystal of 2,6-di-tert-butyl-4-methylphenol in 4 mL of N,N-dimethylformamide was heated at 125° C. under argon for 3 hours. The reaction mixture was then cooled to room temperature, diluted with water, and extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, dried (magnesium sulfate), and concentrated to give a yellow oil. Purification by flash chromatography, eluting with ethyl acetate/hexanes, and recrystallization (ethyl acetate/hexanes) provided the 0.5 g of the title compound as yellow crystals, m.p. 150° C.

1. temperatureThe reaction mixture was then cooled to room temperature
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with saturated aqueous sodium chloride
4. dry with materialdried (magnesium sulfate)
5. concentrationconcentrated
6. customto give a yellow oil
7. customPurification by flash chromatography
8. washeluting with ethyl acetate/hexanes, and recrystallization (ethyl acetate/hexanes)