反应详情

温度

90 °C

A mixture of 2-(4-(2,6-Difluorobenzyloxy)phenyl)acetonitrile (Step A, 5 g, 19.3 mmol), sodium azide (1.3 g, 20 mmol), and ammonium chloride (1.06 g, 20 mmol) in dry DMF (60 ml) was heated at 90° C. for 16 hours. The solvent was removed in vacuo and the oily residue was partitioned between EtOAc and water (acidified to pH 1 with conc. HCl). The organic layer was washed with water, dried over Na2SO4, filtered and concentrated to a brown semisolid. The purification was done by flash chromatography on silica gel column (chloroform:methanol, 9:1) to provide the title compound as a light creamy solid.

1. customThe solvent was removed in vacuo
2. customthe oily residue was partitioned between EtOAc and water (acidified to pH 1 with conc. HCl)
3. washThe organic layer was washed with water
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated to a brown semisolid
7. customThe purification