反应详情

温度

150 °C

##STR8## 1-Nonyne (5.0 g) and Me3SiN3 (6.2 g) were sealed into a heavy-walled glass reactor at -70° C. and 0.6 mm Hg. The mixture was heated at 150° C. for 34 hours, cooled and dissolved in Et2O. The Et2O solution was washed successively with 5 percent aq. HCl, 7 percent aq. NaHCO3, saturated aq. NaCl, dried over MgSO4, filtered and distilled to give 3.89 g (58%) pale yellow oil, bp 110-130/0.05 mm whose NMR spectrum and elemental analysis confirm its structure.

1. temperaturecooled
2. washThe Et2O solution was washed successively with 5 percent aq. HCl, 7 percent aq. NaHCO3, saturated aq. NaCl
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. distillationdistilled
6. customto give 3.89 g (58%)