反应详情

温度

100 °C

The pseudocumene layer from alkylation, containing 0.35-0.38 mole of 3-trifluoropropylamino-4-methylphenol was refluxed in a 1 L 3-necked flask fitted with thermometer, stirrer and Dean-Stark trap in order to remove water as the azeotrope. To the dry solution was added 30 g of phthalic anhydride. Condensation was effected by heating at reflux for 20 hours while removing water generated by reaction as the pseudocumene-water azeotrope. The solution turned red. When condensation was complete the solution was cooled to 100° C., 300 ml water and 25 g 50% sodium hydroxide added, and the pseudocumene removed by azeotropic distillation. The red dye which had crystallized out was separated by filtration and washed with 400 ml water (142 g wet paste). This filtercake was reslurried in 400 ml water and 10 g 50% sodium hydroxide, heated 30 minutes at 100° C., filtered again and washed with 400 ml water. Upon drying at 100° C., 40 g of dye zwitterion was obtained which melted at 258°-260° C.

1. temperaturewas refluxed in a 1 L 3-necked flask
2. customfitted with thermometer, stirrer and Dean-Stark trap in order
3. customto remove water as the azeotrope
4. additionTo the dry solution was added 30 g of phthalic anhydride
5. customCondensation
6. temperatureby heating
7. temperatureat reflux for 20 hours
8. customwhile removing water
9. customgenerated by reaction as the pseudocumene-water azeotrope
10. customWhen condensation
11. customthe pseudocumene removed by azeotropic distillation
12. customThe red dye which had crystallized out
13. customwas separated by filtration
14. washwashed with 400 ml water (142 g wet paste)
15. temperature10 g 50% sodium hydroxide, heated 30 minutes at 100° C.
16. filtrationfiltered again
17. washwashed with 400 ml water
18. customUpon drying at 100° C.
19. custom40 g of dye zwitterion was obtained which melted at 258°-260° C.