反应详情

A stirred mixture of compound 68 (15.00 g, 0.039 mol), 2-methylbut-3-yn-2-ol (7.15 g, 0.085 mol), copper(I) iodide (0.34 g, 1.80 mmol), tetrakis(triphenylphosphine)palladium(0) (2.89 g, 2.50 mmol) and diisopropylamine (150 ml) was heated under reflux in a dry nitrogen atmosphere for 24 h. The resultant mass was dissolved in THF and filtered over hyflo filter aid to remove inorganic materials. Volatile materials were removed in vacuo and the brown solid was recrystallised from ethanol to give a white, fluffy solid.

1. temperaturewas heated
2. temperatureunder reflux in a dry nitrogen atmosphere for 24 h
3. filtrationfiltered over hyflo
4. filtrationfilter aid
5. customto remove inorganic materials
6. customVolatile materials were removed in vacuo
7. customthe brown solid was recrystallised from ethanol
8. customto give a white, fluffy solid