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

HRID 541141
ノート
印刷プレビュー

反応式

HRID 541141 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
180 °C

実験手順

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%).

後処理

  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.

出典と根拠

ORDレコード
ord-2043454e680f4f069c7a3563251f3018
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08871934B2

反応ノート

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