Phthalic Anhydride → N-Butylphthalimide

温度

200 °C

A 10-gallon stainless steel reactor equipped with a turbine blade impeller, cooling coil, distilling condenser, azeotropic separator, thermocouple probe and means to maintain a nitrogen atmosphere, was charged with 15.335 kg (103.53 moles) phthalic anhydride. N-butylamine (7.663 kg, 104.57 moles) from a pressure vessel was slowly added to the reactor which was at room temperature, e.g., about 25° C. The resulting exothermic reaction between the amine and phthalic anhydride was continued until the temperature in the reactor rose to 90° C., at which time addition of amine was complete. The reaction mixture was then heated, with removal of water, for a 5 hour period until the temperature of the mixture reached 200° C. The reaction mixture then was maintained at 200° C. for 2 hours. The resulting product was vacuum distilled at a temperature ranging from 150°-155° C. and at a pressure of 20 mm, to afford a liquid which solidified. The melting point of the solid was about 34° to 35° C. and was produced at a 95% yield.

1. customA 10-gallon stainless steel reactor equipped with a turbine blade impeller
2. temperaturecooling coil
3. distillationdistilling condenser
4. temperatureto maintain a nitrogen atmosphere
5. customwas at room temperature
6. custome.g., about 25° C
7. customreached 200° C
8. distillationdistilled at a temperature
9. customranging from 150°-155° C. and at a pressure of 20 mm
10. customto afford a liquid which
11. customwas about 34° to 35° C.
12. customwas produced at a 95% yield

ORDレコード

ord-e8b93cade60547d195d41db0aafb6404

出典データセット

uspto-grants-1998_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05719295