Phthalic Anhydride → N-Butylphthalimide

HRID 1585224

반응식

HRID 1585224 반응식
[C:1]1(=[O:11])[O:6][C:4](=O)[C:3]2=[CH:7][CH:8]=[CH:9][CH:10]=[C:2]12.[CH2:12]([NH2:16])[CH2:13][CH2:14][CH3:15]>O>[CH2:12]([N:16]1[C:1](=[O:11])[C:2]2=[CH:10][CH:9]=[CH:8][CH:7]=[C:3]2[C:4]1=[O:6])[CH2:13][CH2:14][CH3:15]

참가 물질

4

반응물 2

HCID 6811Phthalic Anhydride2회HCID 8007Butylamine

생성물 1

HCID 73812N-Butylphthalimide수율 95%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
200 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-92bb4be66de74bfcb3e5e729e516418c
출처 데이터셋
uspto-grants-1999_08
특허 번호
US05936099

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