反应详情

温度

100 °C

To a stirred solution of phenylacetylene (1.098 ml, 10 mmol) in abs. toluene (10 ml) was added azidotrimethylsilane (2.65 ml, 20.00 mmol) in one portion. The reaction was heated at 100° C. for 3 days, whereupon was cooled to room temperature and toluene was removed by vacuum. The residue was partitioned between DCM and water. The organic phase was dried over MgSO4 and filtered. After evaporation the crude product was chromatographed in petroleumether:EtOAc=2:1. (Yield: 355 mg, 24%).

1. temperaturewhereupon was cooled to room temperature
2. customtoluene was removed by vacuum
3. customThe residue was partitioned between DCM and water
4. dry with materialThe organic phase was dried over MgSO4
5. filtrationfiltered
6. customAfter evaporation the crude product
7. customwas chromatographed in petroleumether