反应详情

To a stirred slurry of sodium methoxide (1.68 g, 31.25 mmol) in dry THF (15 mL) was added a solution of dimethyl 3-thiahexanedioate (5 g, 26.03 mmol) in THF (10 mL) at rt for 5 min. The reaction mixture was heated at reflux for 2 h, cooled to rt and poured into ice cold water and acidified with dil. HCl. The solution was extracted with chloroform and the combined chloroform layer was washed with water, brine and dried over sodium sulfate. The solution was filtered and evaporated the solvent. The residue was chromatographed over silica gel column using hexane-EtOAc (95:5) as eluents to give the product as pale yellow color oil (1.6 g, 39%).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 2 h
3. additionpoured into ice cold water
4. extractionThe solution was extracted with chloroform
5. washthe combined chloroform layer was washed with water, brine
6. dry with materialdried over sodium sulfate
7. filtrationThe solution was filtered
8. customevaporated the solvent
9. customThe residue was chromatographed over silica gel column