反应详情

温度

50 °C

N-(3-hydroxypropyl)ethylenediamine (19.9 g, 168 mmol), DIPEA (87 mL, 504 mmol, 3.0 eq) were dissolved in 500 mL DMF, followed by the addition of 1,1-carbonyldiimidazole (27.3 g, 168 mmol, 1.0 eq). The reaction was allowed to stir at 50° C. overnight. After overnight, the reaction was cooled to room temperature and TBSCl (25.2 g, 168 mmol, 1.0 eq) was added. The mixture was allowed to stir at room temperature for 3 hours. The reaction was then condensed in vacuo at 40° C. and the obtained residue was then taken into DCM (500 mL). The organic phase was washed with water (2×500 mL) and then with brine (500 mL), dried over MgSO4, filtered and concentrated to afford the title compound as a light yellow solid (42.8 g) in 98% yield.

1. waitAfter overnight
2. temperaturethe reaction was cooled to room temperature
3. stirringto stir at room temperature for 3 hours
4. customcondensed in vacuo at 40° C.
5. washThe organic phase was washed with water (2×500 mL)
6. dry with materialwith brine (500 mL), dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated