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 2248911

반응식

HRID 2248911 반응식
[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](C)(C)CC[Si]([CH2:33][CH2:34][CH2:35][NH2:36])(C)C.N[C:40]1C=CC(OC2C=CC(C(C3C=CC(OC4C=CC(N)=CC=4)=CC=3)(C)C)=CC=2)=C[CH:41]=1.[OH2:70].C[N:72]1[CH2:76][CH2:75][CH2:74][C:73]1=O>C1(C)C(C)=CC=CC=1>[CH3:10][C:9]1([CH3:16])[C:74]2[CH:75]=[C:76]([NH2:72])[CH:40]=[CH:41][C:73]=2[C:7]([C:6]2[CH:33]=[CH:34][C:35]([NH2:36])=[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:70])=[CH:11][C:10]2[C:13]([O:15][C:16](=[O:17])[C:9]=2[CH:8]=1)=[O:14]

참가 물질

7

반응물 5

HCID 962WaterHCID 13387N-methyl-2-pyrrolidone2회HCID 754945,5'-Bi-2-benzofuran-1,1',3,3'-tetroneHCID 831194,4'-(Isopropylidenebis(4,1-phenyleneoxy))dianilineHCID 198804771,2-Bis(gamma-aminopropyldimethylsilyl)ethane

생성물 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)

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

A flask equipped with a stirrer, thermometer, and nitrogen purge 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 69 grams of an N-methyl-2-pyrrolidone solution containing 20.8 grams (0.08 mol) of 1,2-bis(γ-aminopropyldimethylsilyl)ethane 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 52.8 grams of the polyimide resin.

후처리

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

출처 및 근거

ORD 기록
ord-6f25a6181cad413c8aec76ab6bc46091
출처 데이터셋
uspto-grants-1991_08
특허 번호
US05041513

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