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Propyne → Ddsa mthpa

HRID 1976281
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HRID 1976281 반응식
CC#C.C=CC(=C)C.C1(=O)OC(=O)C=C1.[CH3:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25]/[CH:26]=[CH:27]/[CH:28]1[C:33](=[O:34])[O:32][C:30](=[O:31])[CH2:29]1.[CH3:35][C:36]12[C:45](=[O:46])[O:44][C:42](=[O:43])[CH:41]1[CH2:40][CH:39]=[CH:38][CH2:37]2>>[CH3:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25]/[CH:26]=[CH:27]/[CH:28]1[C:33](=[O:34])[O:32][C:30](=[O:31])[CH2:29]1.[CH3:35][C:36]12[C:45](=[O:46])[O:44][C:42](=[O:43])[CH:41]1[CH2:40][CH:39]=[CH:38][CH2:37]2
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참가 물질

6

반응물 5

HCID 6335Propyne2회HCID 6557Isoprene4회HCID 7923Maleic Anhydride2회HCID 198243Methyltetrahydrophthalic anhydrideHCID 6433892Dodecenylsuccinic anhydride

생성물 1

HCID 131722534Ddsa mthpa

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온도
200 °C

실험 절차

The raw materials used in this operation were propylene tetramer supplied by Sunoco or Imperial Oil Esso and isoprene (99.5% pure) was supplied by Goodyear. A 1 L-nitrogen-dried stainless steel Parr reactor, fitted with mechanical stirrer, cooling coils, sampling dip-leg, vent, rupture disk, a pressure sensor, a thermocouple well, and a nitrogen inlet tube was charged with maleic anhydride (86.5 g, 1 eq.) and propylene tetramer (370 g, 2.5 eq.). The vessel was then bolted to the reactor frame and the reaction mixture was purged with nitrogen for 5-10 minutes. The mixture was then heated at 200° C. while stirring at 900 rpm, this stirring being initiated when the reaction temperature had reached 55-60° C., the temperature at which maleic anhydride melts. The pressure built-up in the reactor was monitored with time and temperature (Pmax=39 psi). Sampling was performed during the course of the reaction until the desired conversion (followed by GC) with respect to maleic anhydride was achieved. After the reaction was conducted for 4 hours the reaction mass was cooled to 80° C. by means of external cooling coils on the reactor mantel. Then isoprene (33 g) was introduced through the inlet tube into the reaction mixture. After the isoprene addition, stirring was resumed and the reaction mixture was heated at 100° C. for one hour. The GC analysis showed that no residual maleic anhydride remained in the reaction mixture. The hot reaction mixture was then cooled and the reactor was discharged to a nitrogen-padded sample bottle while venting it with nitrogen. Unreacted starting materials (mostly residual olefin and isoprene) were stripped off under reduced pressure using Kügelrohr equipment. Analysis of the purified light yellow liquid product showed that the product was composed of 83 wt % of DDSA and 17 wt % of MTHPA.

후처리

  1. customA 1 L-nitrogen-dried stainless steel Parr reactor, fitted with mechanical stirrer
  2. temperaturecooling coils
  3. aliquotsampling dip-leg, vent, rupture disk
  4. customthe reaction mixture was purged with nitrogen for 5-10 minutes
  5. customhad reached 55-60° C.
  6. aliquotSampling
  7. customwas performed during the course of the reaction until the desired conversion (followed by GC) with respect to maleic anhydride
  8. temperaturethe reaction mass was cooled to 80° C. by means
  9. temperatureof external cooling coils on the reactor mantel
  10. stirringstirring
  11. temperaturethe reaction mixture was heated at 100° C. for one hour
  12. temperatureThe hot reaction mixture was then cooled

출처 및 근거

ORD 기록
ord-47ec94a7d7bc4b56b95d7e47cf64513a
출처 데이터셋
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06225475B1

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