反应详情

50 mg of copper (I) chloride were dissolved in a mixture of 10 ml of isopropylamine and 15 ml of methanol in an atmosphere of argon, and 660 mg of 3-ethynylanisole were then added to the reaction mixture, followed by stirring at room temperature for 10 minutes. 1300 mg of 1-bromo-3-hydroxy-3-methyl-1-butyne were then dropwisely added to the solution over a time of about 2 hours, followed by stirring at room temperature for 2 hours. The solvent was then evaporated from the reaction mixture, and the residue was then neutralized and diluted by 1N hydrochloric acid, and subjected to extraction with dichloromethane three times. The organic layer was then dried over magnesium sulfate, and the solvent was then evaporated. The residue was then purified by silica-gel column chromatography using benzene as an eluent to obtain 800 mg of 5-hydroxy-5-methyl-1-(3-methoxyphenyl)hexane-1,3-diyne.

1. additionwere then added to the reaction mixture
2. stirringby stirring at room temperature for 2 hours
3. customThe solvent was then evaporated from the reaction mixture
4. additiondiluted by 1N hydrochloric acid
5. extractionsubjected to extraction with dichloromethane three times
6. dry with materialThe organic layer was then dried over magnesium sulfate
7. customthe solvent was then evaporated
8. customThe residue was then purified by silica-gel column chromatography