反应详情

温度

90 °C

tert-butyl 2-azidobenzylcarbamate, 12, (5.4 g, 21.7 mmol) was dissolved in neat propargyl alcohol (10 mL). The reaction mixture was stirred at 90° C. for 18 h. The reaction mixture was then concentrated in vacuo and the resulting residue dissolved in diethyl ether. Upon standing, triazole 13 crystallized. The crystals were collected by filtration yielding 2.5 g (38%) of 13: 1H NMR (400 MHz, CDCl3) δ 7.82, (s, 1H), 7.64-7.35 (m, 3H), 7.34-7.30 (m, 1H), 5.35, (bs, 1H), 4.87, (s, 2H), 4.15 (s, 2H), 1.42 (s, 9H); ESI+ MS: m/z (rel intensity) 249 (100, M-tBu).

1. concentrationThe reaction mixture was then concentrated in vacuo
2. dissolutionthe resulting residue dissolved in diethyl ether
3. customtriazole 13 crystallized
4. filtrationThe crystals were collected by filtration