反应详情

A heavy-walled Pyrex tube was charged with a suspension of N-(3-bromopropyl)phthalimide (1.00 g, 3.72 mmol) and sodium azide (0.32 g, 4.84 mmol) in H2O (2 mL). The tube containing the resulting mixture was sealed with an aluminum crimp cap fitted with a silicon septum and then it was exposed to microwave irradiation for 30 min at a temperature of 120° C. After the irradiation, the reaction tube was cooled with high-pressure air until the temperature had fallen below 40° C. The product was extracted with ethyl acetate. The combined organic layers were dried with magnesium sulfate, filtered and concentrated in vacuo. The crude material (0.62 g, 72% yield) was used without further purification in the next step. 1H NMR (400 MHz, CDCl3) δ 7.86-7.83 (m, 2H), 7.73-7.70 (m, 2H), 3.77 (t, J=6.4 Hz, 2H), 3.36 (t, J=8.0 Hz, 2H), 1.94 (m, 2H).

1. additionThe tube containing the resulting mixture
2. customcap
3. customfitted with a silicon septum
4. customirradiation for 30 min at a temperature of 120° C
5. customAfter the irradiation
6. temperaturethe reaction tube was cooled with high-pressure air until the temperature
7. customhad fallen below 40° C
8. extractionThe product was extracted with ethyl acetate
9. dry with materialThe combined organic layers were dried with magnesium sulfate
10. filtrationfiltered
11. concentrationconcentrated in vacuo