反应详情

Into a reaction flask was weighed 5.6 g of t-BuOK and then 50 ml of THF was added. In 50 ml of DMSO was dissolved 6.2 g of 3,4-methylenedioxyphenol which was then slowly added to the t-BuOK solution with stirring. To the resulting potassium phenate solution was added 10.5 g of 2,5-bis(ethylsulfonyl)pyridine and this mixture heated at 50°-55° C. for 3 hrs. After cooling, the reaction mixture was poured into 400 g of ice, stirred and then filtered. The solid which was recovered was dissolved in CH2Cl2, treated with charcoal, dried over MgSO4 and then filtered. The CH2Cl2 solution was concentrated to 50 ml, diluted with an equal volume of hexane and then chilled and a crystalline material recovered, which provided 9.9 g, (80% yield), of 5-ethylsulfonyl)-2-(3,4-methylenedioxyphenoxy)pyridine, m.p. 97°-99° C.

1. customInto a reaction flask was weighed
2. temperaturethis mixture heated at 50°-55° C. for 3 hrs
3. temperatureAfter cooling
4. stirringstirred
5. filtrationfiltered
6. customThe solid which was recovered
7. dissolutionwas dissolved in CH2Cl2
8. additiontreated with charcoal
9. dry with materialdried over MgSO4
10. filtrationfiltered
11. concentrationThe CH2Cl2 solution was concentrated to 50 ml
12. additiondiluted with an equal volume of hexane
13. temperaturechilled
14. customa crystalline material recovered