反应详情

温度

160 °C

To a solution of 3-cyanonitrobenzene-(20 g, 0.13 mol) in 1-methyl-2-pyrrolidinone (200 ml) was added triethylamine hydrochloride (27.9 g, 0.20 mol) followed by sodium azide (26.4 g, 0.40 mol). The mixture was heated at 160° C. for 1.5 h, then cooled to ambient temperature, poured into ice water (1000 ml) and acidified using 5M HCl. The solid which precipitated from the mixture was filtered, washed with water and dried under vacuum at 50° C. to afford the title tetrazole (22.1 g, 86%) as a beige powder; mp 154°-156° C; δH (360 MHz, CDCl3), 7.59 (1H, t, J=9 Hz), 8.19 (1H, d, J=8 Hz), 8.36 (1H, d, J=8 Hz), 8.86 (1H, s).

1. temperaturecooled to ambient temperature
2. customThe solid which precipitated from the mixture
3. filtrationwas filtered
4. washwashed with water
5. customdried under vacuum at 50° C.