反应详情

温度

90 °C

A mixture of 2-(3-(2,6-Dimethylbenzyloxy)phenyl)acetonitrile (Step B, 3.2 g, 12.7 mmol), sodium azide (1.28 g, 16.7 mmol) and ammonium chloride (1.08 g, 20.2 mmol) in dry dimethylformamide (30 ml) was heated under argon at 90° C. for 9 hours or until all the starting material is consumed and the reaction mixture was concentrated under reduced pressure. The reaction mixture was taken in ethyl acetate and washed with water (2×), dried over Na2SO4, filtered, concentrated and purified by flash chromatography on a silica gel column (methylene chloride:methanol 9:1) to give the oily product. The oil was stirred with 1:2 ethyl acetate:hexane for 10 minutes, and solid was filtered to give product as a white solid.

1. customis consumed
2. concentrationthe reaction mixture was concentrated under reduced pressure
3. washwashed with water (2×)
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. custompurified by flash chromatography on a silica gel column (methylene chloride:methanol 9:1)
8. customto give the oily product
9. filtrationsolid was filtered
10. customto give product as a white solid