反应详情

Chlorosulfonic acid (1.4 ml) was added to 2-(4-pyridyl)thiophene (500 mg) at 0° C. and the mixture was stirred for 5 days at room temperature. Ice-water was carefully added to this mixture at 0° C. to decompose excess reagent. This solution was poured into saturated aqueous NaHCO3 solution (ca. pH 7) and extracted with AcOEt (20 ml×3). The combined organic layer was washed with brine, and dried over MgSO4. After 4N HCl-AcOEt (10 ml) was added to the solution, the solvent was removed in vacuo to give 300 mg of 5-(4-pyridyl)-thiophenesulfonyl chloride as a white solid (yield 32.7%).

1. extractionextracted with AcOEt (20 ml×3)
2. washThe combined organic layer was washed with brine
3. dry with materialdried over MgSO4
4. additionAfter 4N HCl-AcOEt (10 ml) was added to the solution
5. customthe solvent was removed in vacuo