反应详情

(S)—N-(5-(hydroxymethyl)-2,3-dihydro-1H-inden-2-yl)propane-2-sulfonamide (23 mg, 0.086 mmol) was dissolved in DCM (5 mL) and thionyl chloride (51 mg, 0.43 mmol) was added. The reaction mixture was stirred at room temperature for 1 h before being concentrated to dryness. The whole was dissolved in DMF (2 mL) to this was added 3-(trifluoromethyl)-4,5,6,7-tetrahydro-1H-indazole (25 mg, 0.086 mmol) followed by potassium carbonate (24 mg, 0.172 mmol). The reaction mixture was heated to 65° C. for 3 h before being quenched with water (2 mL) and the organics extracted with EtOAc (3×5 mL). The combined organics were washed with brine, dried (MgSO4) and concentrated under reduced pressure. Purification by preparative basic HPLC gave the title compound (1.2 mg, 2.7 μmol, 2.9%). MS (ESI): m/z [M+H]+ 442.2

1. concentrationbefore being concentrated to dryness
2. dissolutionThe whole was dissolved in DMF (2 mL) to
3. temperatureThe reaction mixture was heated to 65° C. for 3 h
4. custombefore being quenched with water (2 mL)
5. extractionthe organics extracted with EtOAc (3×5 mL)
6. washThe combined organics were washed with brine
7. dry with materialdried (MgSO4)
8. concentrationconcentrated under reduced pressure
9. customPurification by preparative basic HPLC