反应详情

Azide 5 (4.66 g, 10.17 mmol) was dissolved in 4 N HCl in dioxane (200 mL), and the solution was stirred at room temperature for 5 h. Solvent was removed under reduced pressure, and the residue was dissolved in water (15 mL) and purified by cation-exchange chromatography (Dowex 50WX8-200 ion-exchange resin, 1 M NH4OH) to give H2NNHCH2CONHCH2CH2N3 as a yellow oil (1.52 g, 95%). HRMS (ESI) [M+Na]+ calcd for C4H10N6ONa, 181.0814; found, 181.0805; 1H NMR (300 MHz, d6-DMSO) δ 8.03 (app bs, 1H), 3.80-3.40 (bs, 3H), 3.40-3.34 (m, 2H), 3.32-3.24 (m, 2H), 3.16 (s, 2H); 13C NMR (75 MHz, d6-DMSO) δ 171.2, 57.1, 50.0, 37.8.

1. customSolvent was removed under reduced pressure
2. dissolutionthe residue was dissolved in water (15 mL)
3. custompurified by cation-exchange chromatography (Dowex 50WX8-200 ion-exchange resin, 1 M NH4OH)