反应详情

温度

120 °C

To a stirred mixture of N-methyl-1,3-diaminopropane (1.70 mL, 16.3 mmol) in pyridine (20 mL) was added sulfamide (1.877 g, 19.5 mmol). The mixture was heated in an oil bath at 120° C. for 16 hrs. After cooling to room temperature, the mixture was concentrated and the residue partitioned between ethyl acetate and saturated aqueous sodium chloride. The organic layer was washed with 1N aqueous hydrochloric acid, saturated aqueous sodium chloride, dried (anhydrous sodium sulfate, filtered, and concentrated to afford a colorless oil (1.3 g, 53%). 1H NMR (300 MHz, CDCl3) δ 4.11 (br s, 1H), 3.60-3.48 (m, 2H), 3.32 (t, 2H, J=5.7 Hz), 2.78 (s, 3H), 1.85-1.72 (m, 2H).

1. temperatureAfter cooling to room temperature
2. concentrationthe mixture was concentrated
3. customthe residue partitioned between ethyl acetate and saturated aqueous sodium chloride
4. washThe organic layer was washed with 1N aqueous hydrochloric acid, saturated aqueous sodium chloride
5. dry with materialdried (anhydrous sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated