Water → 5,5'-Carbonyldi(2-benzofuran-1,3-dione)--1-(4-aminophenyl)-1,3,3-trimethyl-2,3-dihydro-1H-inden-5-amine (1/1)

HRID 373743

Reaktionsgleichung

Reaktionsgleichung von HRID 373743
[CH:1]1[C:6]([C:7]2[CH:12]=[CH:11][C:10]3[C:13]([O:15][C:16](=[O:17])[C:9]=3[CH:8]=2)=[O:14])=[CH:5][C:4]2[C:18]([O:20][C:21](=[O:22])[C:3]=2[CH:2]=1)=[O:19].[CH3:23][N:24]1[CH2:28][CH2:27][CH2:26][C:25]1=O.[OH2:30].C(O[C:35](=O)[CH3:36])(=O)C.[N:38]1C=CC=CC=1>CO>[CH3:18][C:4]1([CH3:3])[C:12]2[CH:11]=[C:10]([NH2:38])[CH:9]=[CH:8][C:7]=2[C:6]([C:25]2[CH:26]=[CH:27][C:28]([NH2:24])=[CH:36][CH:35]=2)([CH3:1])[CH2:5]1.[CH:23]1[C:12]([C:7]([C:6]2[CH:1]=[CH:2][C:3]3[C:21]([O:20][C:18](=[O:19])[C:4]=3[CH:5]=2)=[O:22])=[O:30])=[CH:11][C:10]2[C:13]([O:15][C:16](=[O:17])[C:9]=2[CH:8]=1)=[O:14]

Komponenten

7

Edukt 5

HCID 962WaterHCID 1049PyridineHCID 7918Acetic AnhydrideHCID 13387N-methyl-2-pyrrolidoneHCID 754945,5'-Bi-2-benzofuran-1,1',3,3'-tetrone

Produkt 1

HCID 64544855,5'-Carbonyldi(2-benzofuran-1,3-dione)--1-(4-aminophenyl)-1,3,3-trimethyl-2,3-dihydro-1H-inden-5-amine (1/1)

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

Into a four-neck flask equipped with a thermometer, a stirrer, and a nitrogen introducing tube charged were 10.711 g (0.0364 mol) of 3,3',4,4'-biphenyltetracarboxylic dianhydride, 7.289 g (0.0364 mol) of 2,4'-diaminodiphenyl ether, and 72 g of N-methylpyrrolidone while gaseous nitrogen was passed through the flask. With stirring, reaction was allowed to proceed at room temperature for 10 hours. Due to the formation of polyamic acids having a high molecular weight, the viscosity of the reaction system increased to such a degree that stirring became difficult. After addition of a small amount of water for controlling the molecular weight, the reaction mixture was heated at 60° C. After addition of 52 g of acetic anhydride and 26 g of pyridine, the resulting mixture was allowed to stand for 12 hours at room temperature. The obtained paste was introduced into methanol, and the precipitated fine particles of a solid resin were collected. After sufficiently washed by boiling it in methanol, the solid resin was dried under a reduced pressure at 80° C. for 10 hours, to obtain a powdery polyimide resin (reduced viscosity: 0.68 dl/g) having the repeating unit represented by the following formula.

Aufarbeitung

  1. customInto a four-neck flask equipped with a thermometer, a stirrer, and a nitrogen introducing tube
  2. additioncharged
  3. customreaction
  4. temperaturethe viscosity of the reaction system increased to such a degree
  5. stirringthat stirring
  6. waitto stand for 12 hours at room temperature
  7. customthe precipitated fine particles of a solid resin were collected
  8. washAfter sufficiently washed
  9. customthe solid resin was dried under a reduced pressure at 80° C. for 10 hours

Quellen und Nachweise

ORD-Eintrag
ord-1f5a8232e227491e950fb2247c98bcbe
Quelldatensatz
uspto-grants-1992_11
Patentnummer
US05164816

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