反应详情

温度

60 °C

To a solution of 3-(2-Fluoro-4-iodo-phenylamino)-isonicotinic acid hydrazide (744 mg, 2.ommol) in methanol (15 mL) were added dithiomethane (0.22 mL, 4.66 mmol), followed by potassium hydroxide (2.51 mL, 2.13 mmol). The reaction mixture was stirred at 60° C. for 7 h. The solvent was evaporated and the residue was dissolved in ethyl acetate (50 mL), washed with Brine (15 mL×3), dried over anhydrous MgSO4, filtered, removed off solvent. Residue was subjected to silica gel column (EtOAc:Hexane=1:1) collected product 210 mg. LC-MS (Method A) [5.71 min; 415(M+1)]

1. customThe solvent was evaporated
2. dissolutionthe residue was dissolved in ethyl acetate (50 mL)
3. washwashed with Brine (15 mL×3)
4. dry with materialdried over anhydrous MgSO4
5. filtrationfiltered
6. customremoved off solvent
7. customcollected product 210 mg
8. customLC-MS (Method A) [5.71 min; 415(M+1)]