反应详情

To a stirred solution of 24 (2.2 g, 9.6 mmol) in THF (20 mL) under nitrogen at RT was added diphenylphosphoryl azide (3.96 g, 14.4 mmol) and DIPEA (5 mL). The reaction was stirred for 18 h then diluted with DCM (200 mL) and water (50 mL). The organic layer was dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by SiO2 chromatography eluting with petroleum ether/EtOAc (2:1) to afford 1.2 g (48%) of 5-(azidomethyl)-1-(tetrahydro-2H-pyran-2-yl)-1H-benzo[d]imidazole (26) as yellow oil: MS (ESI) m/z=258.2 [M+1]+.

1. dry with materialThe organic layer was dried (MgSO4)
2. filtrationfiltered
3. concentrationconcentrated in vacuo
4. customThe residue was purified by SiO2 chromatography
5. washeluting with petroleum ether/EtOAc (2:1)