反应详情

温度

70 °C

Tin (II) chloride hydrate (678 mg, 5 eq) was added to a solution of tert-butyl 4-((2-(5-cyanopyrazin-2-ylamino)-5-nitropyridin-4-ylamino)methyl)piperidine-1-carboxylate (273 mg) in ethanol (20 mL). The mixture was heated at 70° C. for 30 minutes then cooled to room temperature and evaporated to dryness. The residue was diluted with ethyl acetate and saturated aqueous sodium hydrogen carbonate. The suspension was filtered and the aqueous phase was separated and extracted twice with ethyl acetate. The combined organic layers were dried (Na2SO4) and concentrated to give crude tert-butyl 4-((5-amino-2-(5-cyanopyrazin-2-ylamino)pyridin-4-ylamino)methyl)piperidine-1-carboxylate (233 mg) as a yellow solid.

1. temperaturethen cooled to room temperature
2. customevaporated to dryness
3. additionThe residue was diluted with ethyl acetate and saturated aqueous sodium hydrogen carbonate
4. filtrationThe suspension was filtered
5. customthe aqueous phase was separated
6. extractionextracted twice with ethyl acetate
7. dry with materialThe combined organic layers were dried (Na2SO4)
8. concentrationconcentrated