反应详情

温度

70 °C

Tin(II)chloride dihydrate (1.59 g, 7.04 mmol) was added portionwise to 5-(4-(4-methoxybenzylamino)-5-nitropyridin-2-ylamino)pyrazine-2-carbonitrile (531 mg, 1.41 mmol) in absolute EtOH (10 mL) at room temperature. The mixture was heated at 70° C. for 2 hours before being concentrated in vacuo. The residue was suspended in a mixture of ethyl acetate and saturated sodium bicarbonate solution, then filtered to remove insoluble material. The solids were then washed with EtOAc. The aqueous phase was re-extracted with ethyl acetate and the combined organic extracts were washed with brine, dried (Na2SO4) and concentrated to give crude title compound (415 mg) as a brown solid. The product was 50% pure by LCMS analysis and was used without further purification. LCMS (2) Rt=1.73 min; m/z (ESI−) 346 (M−H); (ESI+) 348 (MH+).

1. concentrationbefore being concentrated in vacuo
2. additionThe residue was suspended in a mixture of ethyl acetate and saturated sodium bicarbonate solution
3. filtrationfiltered
4. customto remove insoluble material
5. washThe solids were then washed with EtOAc
6. extractionThe aqueous phase was re-extracted with ethyl acetate
7. washthe combined organic extracts were washed with brine
8. dry with materialdried (Na2SO4)
9. concentrationconcentrated