反应详情

A mixture of (S)-3-(1-(2-mercapto-3-nitropyridin-4-ylamino)ethyl)-2-phenyl-8-(trifluoro methyl)isoquinolin-1(2H)-one III-34 (120 mg, 0.247 mmol, 1.0 eq) and stannous chloride dihydrate (297 mg, 1.32 mmol, 5.3 eq) in EtOH (5 mL) was stirred at refluxed for 2 h. The resulting mixture was cooled to RT and concentrated in vacuo. The residue was suspended in water (5 mL), neutralized with saturated NaHCO3 solution to adjust the pH to 7-8 and then extracted with ethyl acetate (5 mL×3). The combined organic layers were washed with brine, dried over Na2SO4 and filtered. The filtrate was concentrated in vacuo to afford the product, (S)-3-(1-(3-amino-2-mercaptopyridin-4-ylamino)ethyl)-2-phenyl-8-(trifluoromethyl)isoquinolin-1(2H)-one III-35.

1. temperatureat refluxed for 2 h
2. concentrationconcentrated in vacuo
3. extractionextracted with ethyl acetate (5 mL×3)
4. washThe combined organic layers were washed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationThe filtrate was concentrated in vacuo