反应详情

温度

120 °C

To a solution of 4-(4-chlorophenyl)-2-methanesulfonyloxy-3-phenylbutane (Step F, 12 g, 34 mmol) in dimethylformamide (50 mL) was added sodium azide (11 g, 0.17 mol). After stirring at 120° C. for 1 h, the reaction mixture was poured into water (200 mL), and the product was extracted with ether (2×100 mL). The combined organic extracts were washed with water, dried over magnesium sulfate, filtered and concentrated to dryness, and the residue was purified on a silica gel column eluting with hexane to 2% ethyl acetate in hexane give the title compound.

1. extractionthe product was extracted with ether (2×100 mL)
2. washThe combined organic extracts were washed with water
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated to dryness
6. customthe residue was purified on a silica gel column
7. washeluting with hexane to 2% ethyl acetate in hexane