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 1885367

Reaktionsgleichung

Reaktionsgleichung von HRID 1885367
[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].N[CH2:24]CC[Si]([CH2:34][CH2:35][CH2:36][NH2:37])(C)O[Si](C)(C)C.N[C:39]1C=CC(OC2C=CC(C(C3C=CC(OC4C=CC(N)=CC=4)=CC=3)(C)C)=CC=2)=C[CH:40]=1.[OH2:69].C[N:71]1[CH2:75][CH2:74][CH2:73][C:72]1=O>C1(C)C(C)=CC=CC=1>[CH3:10][C:9]1([CH3:16])[C:73]2[CH:74]=[C:75]([NH2:71])[CH:39]=[CH:40][C:72]=2[C:7]([C:6]2[CH:34]=[CH:35][C:36]([NH2:37])=[CH:4][CH:5]=2)([CH3:12])[CH2:8]1.[CH:24]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:69])=[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 13387N-methyl-2-pyrrolidone2×HCID 754945,5'-Bi-2-benzofuran-1,1',3,3'-tetroneHCID 831194,4'-(Isopropylidenebis(4,1-phenyleneoxy))dianilineHCID 21585087Bis(aminopropyl)tetramethyldisiloxane

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 7237O-XyleneLösungsmittel

Versuchsvorschrift

A flask equipped with a stirrer, thermometer, and nitrogen inlet tube was charged with 4.4 grams (0.01 mol) of 2,2-bis(3,4-benzenedicarboxylic anhydride)perfluoropropane and 26.5 grams (0.09 mol) of 3,3',4,4'-biphenyltetracarboxylic dianhydride as a tetracarboxylic dianhydride component and 400 grams of N-methyl-2-pyrrolidone as a solvent. To the flask was added dropwise an N-methyl-2-pyrrolidone solution containing 19.8 grams (0.08 mol) of bis(3-aminopropyl)tetramethyldisiloxane and 8.2 grams (0.02 mol) of 2,2-bis[4-(4-aminophenoxy)phenyl]propane as a diamine component while the temperature of the reaction system was controlled so as not to exceed 50° C. After dropwise addition, the reaction mixture was stirred for a further ten hours at room temperature. Then the flask was equipped with a reflux condenser connected to a water collecting container and 30 grams of xylene was added to the flask. The reaction system was heated to 160° C. and maintained at the temperature for four hours to effect reaction. There was obtained a polyimide resin solution which was yellowish brown and clear. During the reaction, 3.4 grams of water formed as a by-product. The polyimide resin solution was poured into methanol from which the polyimide resin was precipitated again and isolated. Vacuum drying at 60° C. for 24 hours yielded 52.6 grams of a polyimide resin.

Aufarbeitung

  1. customA flask equipped with a stirrer
  2. customto exceed 50° C
  3. additionAfter dropwise addition
  4. customThen the flask was equipped with a reflux condenser
  5. additionwas added to the flask
  6. temperatureThe reaction system was heated to 160° C.
  7. temperaturemaintained at the temperature for four hours
  8. customreaction

Quellen und Nachweise

ORD-Eintrag
ord-692378d4c5c04a8699dc30ad3d859263
Quelldatensatz
uspto-grants-1992_09
Patentnummer
US05143948

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