反应详情

温度

100 °C

To a solution of 5,11-dihydro-11-ethyl-8-iodo-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (0.3 g, 0.79 mmol), bis(triphenylphosphine)palladium(II) chloride (18 mg, 0.03 mmol), and 2,6-di-tert-butyl-4-methylphenol (1 crystal) in 5 mL of N,N-dimethylformamide was added benzyltributylstannane (0.36 g, 0.94 mmol). The resultant reaction mixture was heated at 100° C. under argon for 5 hours. An aqueous solution of potassium fluoride was added and the mixture was stirred for 5 hours. The product was extracted with dichloromethane and purified by flash chromatography, eluting with ethyl acetate/dichloromethane, to give 20 mg of the title compound as an oil.

1. customThe resultant reaction mixture
2. extractionThe product was extracted with dichloromethane
3. custompurified by flash chromatography
4. washeluting with ethyl acetate/dichloromethane