반응식
C[C:2]1[CH:7]=[C:6](N)[C:5]([CH3:9])=[CH:4][C:3]=1N.N[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>>[CH:13]1[C:14]2[CH2:15][C:6]3[C:5](=[CH:4][CH:3]=[CH:2][CH:7]=3)[C:9]=2[CH:16]=[CH:17][CH:12]=1참가 물질
실험 절차
In the following Examples, 9,9-bis(3-methyl-4-aminophenyl)fluorene (OTBAF) was prepared as described in U.S. Pat. No. 4,684,678, Example 2. It was recrystallized from anhydrous dichloroethane prior to use. p-Phenylenediamine (PDA) was obtained in a sublimed, zone-refined form from Aldrich Chemical Company. 2,5-Dimethyl(p-phenylenediamine) (DMPDA) was obtained from Aldrich and recrystallized from absolute ethanol prior to use. 4,4'-(1,4-Phenylenebis(1-methylethylidene))bisbenzamine (EHPT) was obtained from Shell Chemical Company and was recrystallized from anhydrous dichloroethane prior to use. 9,9-Bis((3,5-dimethyl-4-amino)phenyl)fluorene (DM-OTBAF), 9,9-Bis[(3-ethyl-5-methyl-4-amino)phenyl)]fluorene (DE-OTBAF), and 9,9-bis[(2,5-diethyl-4-amino)phenyl]fluorene (DEAF) were prepared analogously, but using a different aniline derivative, as OTBAF, and were recrystallized prior to use. 3,3'-4,4'-Benzophenone tetracarboxylic acid dianhydride (BTDA) was purchased from Aldrich in a sublimed form. 4,4'-Oxydi(phthalic anhydride) (ODPA) was obtained from Occidental Chemical Company and purified via recrystallization from anisole. Pyromellitic dianhydride (PMDA), 2,2'-bis-((3,4-dicarboxyphenyl)-hexafluoropropane dianhydride (6FDA), 3,3'-4,4'-biphenyltetracarboxylic dianhydride (s-BPDA), and DSDA (3,3'-4,4'-diphenyl sulfone tetracarboxylic acid dianhydride) were purchased and used as received from Chriskev Company of Leawood, Kans.
후처리
- customrecrystallized from absolute ethanol
- customwas recrystallized from anhydrous dichloroethane
- customas OTBAF, and were recrystallized
- custompurified via recrystallization from anisole
출처 및 근거
- ORD 기록
- ord-24d58cc2f3c94cc8b0496e38c9d3de1c
- 출처 데이터셋
- uspto-grants-1999_10
- 특허 번호
- US05969088
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