反应详情

温度

5 °C

A solution of phthalimide 303 (5.96 g, 21.0 mmol) and N2H4.H2O (2.04 mL, 42.0 mmol in EtOH (60 mL) was stirred at reflux temperature for 2 h. The solution was cooled to 5° C. for 2 h, the precipitate filtered, washed with EtOH (5 mL) and the filtrate evaporated to half volume. The solution was cooled at 5° C. for a further 2 h, the precipitate filtered, washed with EtOH (5 mL) and the filtrate evaporated to give diamine 304 which was used without further purification: 1H NMR δ 2.94-3.02 (m, 1H, CHCN), 2.90 (dd, J=9.0, 7.9 Hz, 1H, CH2), 2.82 (t, J=6.8 Hz, 2H, CH2N), 2.61-2.68 (m, 2H, CH2N), 2.48-2.58 (m, 3H, CH2N), 2.05-2.15 (m, 1H, CH2), 2.03-2.11 (m, 1H, CH2), 1.68 (p, J=7.0 Hz, 2H, CH2), NH2 not observed.

1. temperatureat reflux temperature for 2 h
2. filtrationthe precipitate filtered
3. washwashed with EtOH (5 mL)
4. customthe filtrate evaporated to half volume
5. temperatureThe solution was cooled at 5° C. for a further 2 h
6. filtrationthe precipitate filtered
7. washwashed with EtOH (5 mL)
8. customthe filtrate evaporated