反应 #2021468

反应方程式

2,5-Dimethyl(p-phenylenediamine)

aniline

→

fluorene

反应条件

后处理

1. 1
   其他recrystallized from absolute ethanol
2. 2
   其他was recrystallized from anhydrous dichloroethane
3. 3
   其他as OTBAF, and were recrystallized
4. 4
   其他purified via recrystallization from anisole

实验过程

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.

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