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温度

0 °C

To a solution of 6-(5-aminomethyl-pyridin-3-yl)-1-methyl-3,4-dihydro-1H-quinolin-2-one (example 36, 0.05 g, 0.187 mmol) in DCM (1 mL) cooled to 0° C. were added triethylamine (0.038 g, 0.374 mmol) and isopropylsulfonylchloride (0.029 g, 0.206 mmol). The resulting suspension was stirred at 0° C. for 4 h and then allowed to warm up to room temperature and stirring was continued for 2 h. The reaction mixture was diluted with DCM, poured into H2O (5 mL) and extracted with DCM (2×10 mL). Combined organics were dried over Na2SO4, filtered and evaporated to dryness. The residue was purified by silica gel flash chromatography eluting with a 0 to 10% MeOH(1% NH4OH)-DCM gradient to give the title compound (0.023 g, 33%) as a white foam. MS: 374.1 (M+H+).

1. temperatureto warm up to room temperature
2. stirringstirring
3. waitwas continued for 2 h
4. extractionextracted with DCM (2×10 mL)
5. dry with materialCombined organics were dried over Na2SO4
6. filtrationfiltered
7. customevaporated to dryness
8. customThe residue was purified by silica gel flash chromatography
9. washeluting with a 0 to 10% MeOH(1% NH4OH)-DCM gradient