反应详情

温度

150 °C

Triethylamine hydrochloride (41.25 g, 0.3 mol) and sodium azide (39 g, 0.6 mol) were added to a solution of 4-nitrophenylacetonitrile (32.4 g, 0.2 mmol) in anhydrous N-methylpyrrolidin-2-one (500 ml) and the mixture heated at 150° C. for 4h. The solution was cooled to room temperature and poured into 2N HCl (2 l) whereupon a solid crystallised out. The product was filtered, washed with water (500 ml) and hexane and dried in vacuo (37.4 g); δ (250 MHz, CDCl3) 4.34 (2H, s, CH2), 7.42 (2H, d, J=8.7 Hz, Ar--H), 8.12 (2H, d, J=8.7 Hz, Ar--H).

1. temperatureThe solution was cooled to room temperature
2. customcrystallised out
3. filtrationThe product was filtered
4. washwashed with water (500 ml) and hexane
5. customdried in vacuo (37.4 g)