Trimethylolpropane → Abietic Acid

HRID 430723

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HRID 430723 반응식
[CH2:1]([C:3]([CH2:8]O)([CH2:6][OH:7])[CH2:4][CH3:5])O.[C:10]1(O)[C:11](=[CH:13][C:14](=[CH:16][CH:17]=1)O)[CH3:12].[OH-:19].[K+]>>[CH3:13][CH:14]([C:14]1[CH2:16][CH2:17][C@H:10]2[C:11](=[CH:12][CH2:5][C@H:4]3[C@@:3]([C:6]([OH:19])=[O:7])([CH3:8])[CH2:1][CH2:12][CH2:11][C@@:10]32[CH3:17])[CH:13]=1)[CH3:16]

참가 물질

4

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온도
125 °C

실험 절차

5 10.26 kg of Portuguese balsam resin WW 4.02 kg of trimethylolpropane and 0.007 kg of toluhydroquinone were weighed into a 15 liter stirred tank equipped with a distillation attachment and nitrogen (30 to 40 l/h) was passed over the mixture for 30 minutes. The stream of nitrogen was reduced to 8 to 10 l/h and the mixture was heated to 120 to 130° C. When the resin had melted, the stirrer Incas switched on. The reaction mixture was subsequently heated to 140° C. over a period of 2 h, and then maintain the following temperatures: 1 h at 140° C., 1 h at 150° C. 1 h at 160° C., 1 h at 170° C., 1 h at 180° C., 1 h at 200° C. and I h at 220° C. The stream of nitrogen was then increased to 20 l/h and the reaction mixture was heated to 230° C. and stirred at this temperature until the acid number was less than 10 mg KOH per g substance.

후처리

  1. customequipped with a distillation attachment and nitrogen (30 to 40 l/h)
  2. temperatureThe reaction mixture was subsequently heated to 140° C. over a period of 2 h
  3. temperaturemaintain the following temperatures
  4. custom1 h
  5. customat 140° C.
  6. custom1 h
  7. customat 150° C
  8. custom1 h
  9. customat 160° C.
  10. custom1 h
  11. customat 170° C.
  12. custom1 h
  13. customat 180° C.
  14. custom1 h
  15. customat 200° C.
  16. customh at 220° C
  17. temperatureThe stream of nitrogen was then increased to 20 l/h
  18. temperaturethe reaction mixture was heated to 230° C.
  19. stirringstirred at this temperature until the acid number

출처 및 근거

ORD 기록
ord-bdfcb9e9749d4b3da83ec667ccb2fec0
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06323254B1

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