反应详情

To a stirred solution of propargylamine hydrochloride (5.0 g, 54.6 mmol) and pyridine (7.8 g, 99.1 mmol) in tetrahydrofuran (30 mL) was added 4-nitro-benzoylchloride (9.2 g, 49.6 mmol) in tetrahydrofuran (20 mL) and the mixture was heated at reflux for 16 h. The mixture was allowed to cool to ambient temperature and concentrated in vacuo. The crude residue was dissolved in ethyl acetate and washed with saturated aqueous sodium bicarbonate solution, water, brine, dried over anhydrous sodium sulphate, filtered and concentrated in vacuo to afford 4-nitro-N-prop-2-ynyl-benzamide (7.74 g, 77%) as a solid.

1. temperaturethe mixture was heated
2. temperatureat reflux for 16 h
3. concentrationconcentrated in vacuo
4. dissolutionThe crude residue was dissolved in ethyl acetate
5. washwashed with saturated aqueous sodium bicarbonate solution, water, brine
6. dry with materialdried over anhydrous sodium sulphate
7. filtrationfiltered
8. concentrationconcentrated in vacuo