反应详情

温度

60 °C

To a solution of methyl 4-(N-(benzofuran-5-ylmethyl)-N-(3-chloro-5-(trifluoromethyl)pyridin-2-yl)sulfamoyl)benzoate (step-2 of Example 1, 2.3 g, 4.3 mmol) in THF (15 mL) was added 2 M aqueous NaOH (9.0 mL) at room temperature, and the mixture was heated at 60° C. for 2 hrs. The mixture was cooled with ice bath, and acidified by the addition of 2 M aqueous HCl (10 mL). The mixture was extracted with DCM (30 mL×2), dried over Na2SO4, filtered and the filtrate was concentrated to give a white solid. The residual solid was triturated with IPE (50 mL), the precipitates were collected by filtration, washed with IPE, and dried in vacuo at 50° C. to give 1.6 g (74% yield) of the titled compound as a white powder.

1. temperatureThe mixture was cooled with ice bath
2. extractionThe mixture was extracted with DCM (30 mL×2)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationthe filtrate was concentrated
6. customto give a white solid
7. customThe residual solid was triturated with IPE (50 mL)
8. filtrationthe precipitates were collected by filtration
9. washwashed with IPE
10. customdried in vacuo at 50° C.