反应详情

温度

0 °C

18 μl (16 mg, 0.29 mmol) of propargylamine, 40 μl (29 mg, 0.29 mmol) of triethylamine and 1 mg (0.01 mmol) of N,N-dimethylaminopyridine were initially charged in 0.5 ml of dichloromethane, and 105 mg (0.29 mmol) of 5-(4-ethylphenyl)-1-(morpholin-4-ylcarbonyl)piperidine-3-carbonyl chloride, dissolved in 1 ml of dichloromethane, were added. The reaction mixture was stirred at 0° C. for 30 minutes and at RT for 16 h. For work-up, water was added and the reaction mixture was extracted with ethyl acetate. The combined organic extracts were dried over magnesium sulphate, filtered and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (mobile phase dichloromethane/methanol 100:5). Yield: 108 mg (98% of theory.)

1. additionwere added
2. extractionthe reaction mixture was extracted with ethyl acetate
3. dry with materialThe combined organic extracts were dried over magnesium sulphate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by column chromatography on silica gel (mobile phase dichloromethane/methanol 100:5)