反应详情

3-Cyclopropyl-prop-2-yn-1-ol (3.28 g, 34.1 mmol) was dissolved in 40 mL toluene, DPPA (11.26 g, 40.9 mmol) was added, followed with DBU (6.24 g, 40.9 mmol) while maintaining temperature with a water bath. The mixture was stirred at room temperature for one hour and was diluted with 100 mL hexane and 15 mL CH2Cl2. The mixture was washed with water four times and once with brine, dried over Na2SO4, filtered and concentrated under rotovap with cold water bath to remove most of organic solvent leaving some toluene (product volatile). The residual oil was used for the next step.

1. temperaturewhile maintaining temperature with a water bath
2. washThe mixture was washed with water four times and once with brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated under rotovap with cold water bath
6. customto remove most of organic solvent
7. customleaving some toluene (product volatile)