反应详情

温度

60 °C

Cinnamic acid (100 gms) and p-cresol (76.6 gms) were charged to a clean and dry flask under nitrogen and stirred. Concentrated sulphuric acid was slowly charged and the reaction mixture heated to 125° C.-130° C. for 6 hours. After completion of reaction the mixture was cooled to about 60° C. and about 50 ml water and about 300 ml toluene were charged under stirring. The layers were separated. The toluene layer was washed with aqueous saturated solution of sodium bicarbonate and water. The organic layer was dried over sodium sulfate and concentrated under vacuum, at a temperature below 50° C. The residue was stripped with 2×100 ml IPA. The residue was dissolved in 200 ml isopropanol, chilled to 5° C. and stirred for 2 hours. The solids obtained were filtered and dried at about 60° C. for 4-5 hours to give about 135 to 137 gms of the title product.

1. customdry flask under nitrogen
2. additionConcentrated sulphuric acid was slowly charged
3. temperaturethe reaction mixture heated to 125° C.-130° C. for 6 hours
4. customAfter completion of reaction the mixture
5. stirringunder stirring
6. customThe layers were separated
7. washThe toluene layer was washed with aqueous saturated solution of sodium bicarbonate and water
8. dry with materialThe organic layer was dried over sodium sulfate
9. concentrationconcentrated under vacuum, at a temperature below 50° C
10. dissolutionThe residue was dissolved in 200 ml isopropanol
11. temperaturechilled to 5° C.
12. stirringstirred for 2 hours
13. customThe solids obtained
14. filtrationwere filtered
15. customdried at about 60° C. for 4-5 hours