反应详情

A solution of thiophenol (70 mmol) in THF (10 ml) was refluxed for 1 h in the presence of K2CO3 (70 mmol) as a base. A solution of Cyclobutylidene acetic acid (intermediate 1) (35 mmol) in DMF (1.0 ml) was added to the above reaction. The reaction was monitored by TLC for completion. After 3 days the reaction was cooled and filtered. It was then neutralized with ethyl acetate saturated with hydrochloric acid and the compound was extracted with ethyl acetate. Organic layer was then separated, dried over anhydrous Na2SO4 and concentrated under vacuum. The residue was column purified to give the compound as a yellow solid.

1. temperatureAfter 3 days the reaction was cooled
2. filtrationfiltered
3. extractionthe compound was extracted with ethyl acetate
4. customOrganic layer was then separated
5. dry with materialdried over anhydrous Na2SO4
6. concentrationconcentrated under vacuum
7. custompurified