反应详情

To a suspension of 4-hydroxymethylimidazole II-1 (1.09 g, 11.1 mmol) in CH3CN (12 mL), SOCl2 (5 mL) was added. After being stirred at room temperature for 30 min, the suspension became clear. After stirring for additional 2 h, the solution was concentrated in vacuo to give a solid, which was then dissolved in DMF (15 mL). To the solution, NaN3 (2.16 g, 33.2 mmol) was added. After the mixture was stirred at room temperature overnight, water and EtOAc were added, then 5% aq. NaHCO3 was also added. The organic layer was separated, dried over Na2SO4, concentrated in vacuo to give 4-azidomethylimidazole as a solid (0.759 g). MS 124.1 (M+H).

1. stirringAfter stirring for additional 2 h
2. concentrationthe solution was concentrated in vacuo
3. customto give a solid, which
4. stirringAfter the mixture was stirred at room temperature overnight
5. customThe organic layer was separated
6. dry with materialdried over Na2SO4
7. concentrationconcentrated in vacuo