反应详情

In 20 ml of ethanol was dissolved 0.11 g of metallic sodium and after adding 1 g of 4,5-diphenyl-2-mercaptoimidazole to the solution followed by stirring several minutes, 1 g of 3,5-di-tert-butylphenacyl bromide was added thereto followed by stirring for one hour at room temperature. The reaction mixture was concentrated udner reduced pressure and then water was added to the residue. The crystals thus formed were recovered by filtration, dried, dissolved in 20 ml of phosphorus oxychloride, and the solution was refluxed for 14 hours. The reaction mixture was concentrated under reduced pressure and after adding water to the residue followed by neutralization with potassium carbonate, the product was extracted with chloroform. The extract was dried and concentrated. The residue was subjected to silica gel column chromatography and the product was eluted with chloroform. The crude crystals thus obtained were recrystallized from ethanol to provide 0.8 g of 3-(3,5-di-tert-butyl-4-hydroxyphenyl)-5,6-diphenyl imidazo[2,1-b]thiazole.

1. stirringby stirring for one hour at room temperature
2. concentrationThe reaction mixture was concentrated udner reduced pressure
3. additionwater was added to the residue
4. customThe crystals thus formed
5. filtrationwere recovered by filtration
6. customdried
7. dissolutiondissolved in 20 ml of phosphorus oxychloride
8. temperaturethe solution was refluxed for 14 hours
9. concentrationThe reaction mixture was concentrated under reduced pressure
10. additionafter adding water to the residue
11. extractionthe product was extracted with chloroform
12. customThe extract was dried
13. concentrationconcentrated
14. washthe product was eluted with chloroform
15. customThe crude crystals thus obtained
16. customwere recrystallized from ethanol