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2'-Methyl-biphenyl-2,4'-dicarboxylic acid → 4-methyl-9-oxo-9H-fluorene-2-carboxylic acid

HRID 1799022
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인쇄 미리보기

반응식

HRID 1799022 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([C:8]([OH:10])=[O:9])[CH:5]=[CH:4][C:3]=1[C:11]1[C:12]([C:17](O)=[O:18])=[CH:13][CH:14]=[CH:15][CH:16]=1>O>[CH3:1][C:2]1[C:3]2[C:11]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:17](=[O:18])[C:4]=2[CH:5]=[C:6]([C:8]([OH:10])=[O:9])[CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 594924972'-Methyl-biphenyl-2,4'-dicarboxylic acid

생성물 1

HCID 594925644-methyl-9-oxo-9H-fluorene-2-carboxylic acid수율 97%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
180 °C

실험 절차

A mixture of 2′-methyl-biphenyl-2,4′-dicarboxylic acid (1.94 g) and polyphosphoric acid (50 g) was stirred at 180° C. for 3 hr. The reaction mixture was cooled to room temperature, water (100 ml) was slowly added dropwise, and the mixture was further stirred at room temperature for 10 min. This suspension was filtered, and the obtained solid was successively washed with water (50 ml) and 50 v/v % aqueous methanol solution (50 ml). The obtained solid was air-dried, and dried under reduced pressure at 80° C. to give the title compound (1.745 g, 97%).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. stirringthe mixture was further stirred at room temperature for 10 min
  3. filtrationThis suspension was filtered
  4. washthe obtained solid was successively washed with water (50 ml) and 50 v/v % aqueous methanol solution (50 ml)
  5. customThe obtained solid was air-dried
  6. customdried under reduced pressure at 80° C.

출처 및 근거

ORD 기록
ord-bde43fa7d41d4710b1696f6d41905484
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08343994B2

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