反应详情

温度

90 °C

A mixture of 2-(3-(2,6-dimethylbenzyloxy)-2-methoxyphenyl)acetonitrile (Step D, 3.2 g, 12.7 mmol), sodium azide (0.86 g, 13.2 mmol) and ammonium chloride (0.696 g, 13.0 mmol) in dry DMF (10 ml) was heated under argon at 90° C. for 16 hours or until all the starting material is consumed, the reaction mixture was cooled, and concentrated under reduced pressure and purified by flash chromatography on a silica gel column (chloroform:methanol 9:1) to give semi solid product. The semi solid was stirred with 1:2 ethyl acetate:hexane (15 ml) for 10 minutes, and filtered to give product as a white solid.

1. customis consumed
2. temperaturethe reaction mixture was cooled
3. concentrationconcentrated under reduced pressure
4. custompurified by flash chromatography on a silica gel column (chloroform:methanol 9:1)
5. customto give semi solid product
6. filtrationfiltered
7. customto give product as a white solid