反应详情

In a 10 mL round-bottomed flask 5-[3-(4-amino-phenyl)-3-(4-chloro-2-methyl-phenyl)-propionyl]-1-methyl-1H-pyridin-2-one (88 mg) and methanesulfonyl chloride (40.1 mg) were combined with pyridine (0.87 mL) to give a brown solution. The reaction mixture was stirred at room temperature for 3 h. The crude reaction mixture was concentrated in vacuo. The reaction mixture was extracted 3× with ethyl acetate, the organic layers were washed 3× with water and dried over magnesium sulfate and concentrated in vacuo. The crude material was purified by flash chromatography (silica gel, 20 g, 0% to 10% methanol in dichloromethane) to give the title compound (68 mg) as a colourless foam, MS (ESI+): m/z=459.3 [M+H]+.

1. customto give a brown solution
2. customThe crude reaction mixture
3. concentrationwas concentrated in vacuo
4. extractionThe reaction mixture was extracted 3× with ethyl acetate
5. washthe organic layers were washed 3× with water
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated in vacuo
8. customThe crude material was purified by flash chromatography (silica gel, 20 g, 0% to 10% methanol in dichloromethane)