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Aniline → Fluorene

HRID 1740332
ノート
印刷プレビュー

反応式

HRID 1740332 の反応式
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]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 6115AnilineHCID 1608242,5-Dimethyl-p-phenylenediamine

生成物 1

HCID 6853Fluorene

実験手順

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.

後処理

  1. customrecrystallized from absolute ethanol
  2. customwas recrystallized from anhydrous dichloroethane
  3. customas OTBAF, and were recrystallized
  4. custompurified via recrystallization from anisole

出典と根拠

ORDレコード
ord-24d58cc2f3c94cc8b0496e38c9d3de1c
出典データセット
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05969088

反応ノート

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