反应详情

温度

150 °C

Palladium(II)acetate (32 mg, 0.14 mmol) was added to (±)-2,2″-bis(diphenylphosphino)-1,1″-binaphthalene (268 mg, 0.4 mmol) in DMF/toluene (1/1) and the resulting mixture was degassed under a stream of nitrogen gas for 10 minutes. 2-Amino-5-cyanopyrazine (172 mg, 1.43 mmol), sodium tert-butoxide (207 mg, 2.15 mmol) and tert-butyl 4-((2-bromo-5-nitropyridin-4-ylamino)methyl)piperidine-1-carboxylate (595 mg, 1.43 mmol) were added and the mixture was degassed for a further 5 minutes before being heated at 150° C. for 30 minutes using microwave irradiation. The mixture was concentrated in vacuo and partially purified by silica chromatography, eluting with 40% ethyl acetate-hexane, to give 273 mg of tert-butyl 4-((2-(5-cyanopyrazin-2-ylamino)-5-nitropyridin-4-ylamino)methyl)piperidine-1-carboxylate at a purity of 75% which was used without further purification.

1. customthe resulting mixture was degassed under a stream of nitrogen gas for 10 minutes
2. customthe mixture was degassed for a further 5 minutes
3. custommicrowave irradiation
4. concentrationThe mixture was concentrated in vacuo
5. custompartially purified by silica chromatography
6. washeluting with 40% ethyl acetate-hexane