反应详情

The crude 5-phenyl-3-(4-piperidinyl)-1H-indazole-7-carboxamide hydrochloride (Example 2) was suspended in DMF (8 mL) and treated with triethylamine (0.3 mL, 2.2 mmols), DMAP (0.0056 g, 0.065 mmol), and ethane sulfonyl chloride (0.044 mL, 0.47 mmols) at ambient temperature. After 12 hrs, the mixture was concentrated to dryness in vacuo at ambient temperature, treated with water (10 mL), and extracted with ethyl acetate (3×25 mL). The organic phase was washed with water, dried over MgSO4, filtered, and concentrated to give a light brown solid. This was purified via preparative HPL, eluting with 10% B to 80% B, where A=H2O (0.1% trifluoroacetic acid) and B=CH3CN (0.1% trifluoroacetic acid) to give 0.080 g of a white solid.

1. concentrationthe mixture was concentrated to dryness in vacuo at ambient temperature
2. additiontreated with water (10 mL)
3. extractionextracted with ethyl acetate (3×25 mL)
4. washThe organic phase was washed with water
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customto give a light brown solid
9. customThis was purified via preparative HPL
10. washeluting with 10% B to 80% B, where A=H2O (0.1% trifluoroacetic acid) and B=CH3CN (0.1% trifluoroacetic acid)