反应详情

温度

80 °C

tert-Butyl[(5-chloro-2-fluoro-4-{2-[3-nitro-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-4-yl]-4-(trifluoromethoxy)phenoxy}phenyl)sulfonyl]1,3-thiazol-4-ylcarbamate (Preparation 25, 3.70 g, 4.84 mmol), and saturated aqueous ammonium chloride solution (17 mL) were added to ethanol (62 mL). A white precipitate formed. Iron (0.541 g, 9.68 mmol) was added and the reaction mixture heated at 80° C. After 2 hours the reaction mixture was cooled, filtered and concentrated in vacuo. The residue was slurried in water and the solid collected by filtration. The solid was rinsed with water, then dissolved in ethyl acetate, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was dissolved in a saturated solution of hydrogen chloride in methanol and heated at 50° C. for 2 hours. The solvent was removed in vacuo and the residue dissolved in a minimum amount of methanol. Ethyl acetate was added and the solution stirred for 4 hours while crystals formed. The solid was collected by filtration to afford the title compound as a white powder (1.75 g).

1. customA white precipitate formed
2. temperatureAfter 2 hours the reaction mixture was cooled
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. filtrationthe solid collected by filtration
6. washThe solid was rinsed with water
7. dissolutiondissolved in ethyl acetate
8. dry with materialdried over anhydrous magnesium sulfate
9. concentrationconcentrated in vacuo
10. dissolutionThe residue was dissolved in a saturated solution of hydrogen chloride in methanol
11. temperatureheated at 50° C. for 2 hours
12. customThe solvent was removed in vacuo
13. dissolutionthe residue dissolved in a minimum amount of methanol
14. additionEthyl acetate was added
15. customformed
16. filtrationThe solid was collected by filtration