反应详情

Method I Combine 6-amino-1-isopropyl-3-(3,4,5-trifluoro-phenyl)-1H-indole (116.6 mg, 0.38 mmol), prepared as described immediately above, dichloromethane (3.0 mL) and pyridine (62 μL, 0.76 mmol) under a nitrogen atmosphere in a 25 mL flask. Cool the reaction to 0° C. and add methane sulfonyl chloride (33 μL, 0.42 mmol). Allow the reaction to warm to RT while stirring for 3 hours. Quench reaction with saturated aqueous sodium bicarbonate (5 mL), dilute with ethyl acetate (10 mL) and separate the layers. Wash the organic layer with water (5 mL), brine (5 mL), dry (Na2SO4) and filter. Concentrate the filtrate and adsorb the crude product onto silica gel. Purify by silica gel chromatography eluting with ethyl acetate in dichloromethane (0-5 v/v %) to give 95.1 mg of the title compound (61%). LRMS (API ES+)=383.0 (M+H).

1. temperatureCool
2. customthe reaction to 0° C.
3. customthe reaction
4. customQuench
5. customreaction with saturated aqueous sodium bicarbonate (5 mL)
6. customseparate the layers
7. washWash the organic layer with water (5 mL), brine (5 mL)
8. dry with materialdry (Na2SO4)
9. filtrationfilter
10. concentrationConcentrate the filtrate
11. customPurify by silica gel chromatography
12. washeluting with ethyl acetate in dichloromethane (0-5 v/v %)