反应详情

After cooling, the reaction liquid was concentrated under reduced pressure, and azeotroped with benzene. A tetrahydrofuran solution (7 ml) of the resulting residue was dropwise added to a tetrahydrofuran solution (63 ml) of 2-amino-5-bromo-4-fluoro-3-hydroxy-6-methylbenzonitrile (I-75) (3.13 g, 12.77 mmol) and sodium hydrogencarbonate (2.68 g, 31.93 mmol), followed by stirring at room temperature for 19 hours. Ethyl acetate was added to the reaction liquid, followed by washing with water and saturated brine. The organic layer was concentrated under reduced pressure, the resulting residue was dissolved in ethanol (30 ml), aqueous 1 N sodium hydroxide solution (24 ml) was added, followed by stirring at 50° C. for 23 hours. After cooling, the reaction liquid was concentrated under reduced pressure, diluted with ethyl acetate, neutralized with aqueous 1 N hydrochloric acid, washed with saturated brine. The organic layer was concentrated under reduced pressure to obtain the entitled compound (5.82 g, 70%) as a yellow white solid.

1. temperatureAfter cooling
2. customthe reaction liquid
3. concentrationwas concentrated under reduced pressure
4. customazeotroped with benzene
5. washby washing with water and saturated brine
6. concentrationThe organic layer was concentrated under reduced pressure
7. dissolutionthe resulting residue was dissolved in ethanol (30 ml)
8. additionaqueous 1 N sodium hydroxide solution (24 ml) was added
9. stirringby stirring at 50° C. for 23 hours
10. temperatureAfter cooling
11. customthe reaction liquid
12. concentrationwas concentrated under reduced pressure
13. additiondiluted with ethyl acetate
14. washwashed with saturated brine
15. concentrationThe organic layer was concentrated under reduced pressure