4-Hydroxyphthalic acid → 9,9-Bis{4-(4-hydroxy-phthalimido)phenyl}fluorene

HRID 1770297노트

반응식

HRID 1770297 반응식
[OH:1][C:2]1[CH:3]=[C:4]([C:11]([OH:13])=O)[C:5](=[CH:9][CH:10]=1)[C:6]([OH:8])=O.[NH2:14][C:15]1[CH:20]=[CH:19][C:18]([C:21]2([C:34]3[CH:39]=[CH:38][C:37]([NH2:40])=[CH:36][CH:35]=3)[C:33]3[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=3[C:27]3[C:22]2=[CH:23][CH:24]=[CH:25][CH:26]=3)=[CH:17][CH:16]=1>C(O)(=O)C>[OH:1][C:2]1[CH:3]=[C:4]2[C:11](=[O:13])[N:14]([C:15]3[CH:16]=[CH:17][C:18]([C:21]4([C:34]5[CH:35]=[CH:36][C:37]([N:40]6[C:11](=[O:13])[C:4]7=[CH:3][C:2]([OH:1])=[CH:10][CH:9]=[C:5]7[C:6]6=[O:8])=[CH:38][CH:39]=5)[C:22]5[CH:23]=[CH:24][CH:25]=[CH:26][C:27]=5[C:28]5[C:33]4=[CH:32][CH:31]=[CH:30][CH:29]=5)=[CH:19][CH:20]=3)[C:6](=[O:8])[C:5]2=[CH:9][CH:10]=1

참가 물질

4

반응물 2

HCID 118814-Hydroxyphthalic acidHCID 6315524,4'-(9-Fluorenylidene)dianiline

생성물 1

HCID 200959569,9-Bis{4-(4-hydroxy-phthalimido)phenyl}fluorene수율 53.1%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 4-hydroxyphthalic acid (4.0 g, 22 mmol), 9,9-bis(4-aminophenyl)fluorene (3.5 g, 10 mmol), and 40 ml of acetic acid was stirred and heated under reflux for 48 hours. After cooling to room temperature, the precipitate was collected by filtration and washed with acetic acid (2×25 ml) to provide the title compound as a colorless powder having a melting point greater than 300° C. (3.4 g, 53.1% yield). The nuclear magnetic resonance and infrared spectrum were consistent with the structure.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 48 hours
  3. filtrationthe precipitate was collected by filtration
  4. washwashed with acetic acid (2×25 ml)

출처 및 근거

ORD 기록
ord-0071074c03bd44e382cd13ba5a8c2091
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05386002

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