9-Oxofluorene-4-carboxylic acid → HCID 59208194、化合物

HRID 2243314

反応式

HRID 2243314 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH-:8].[O:9]=[C:10]1[C:22]2[CH:21]=[CH:20][CH:19]=[C:18]([C:23](O)=O)[C:17]=2[C:16]2[C:11]1=[CH:12][CH:13]=[CH:14][CH:15]=2>C(O)(=O)C>[NH:1]1[C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=2[N:8]=[C:23]1[C:18]1[C:17]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10](=[O:9])[C:22]=2[CH:21]=[CH:20][CH:19]=1

参加物

4

反応物 2

HCID 803619-Oxofluorene-4-carboxylic acidHCID 86621027HCID 86621027、化合物

生成物 1

HCID 59208194HCID 59208194、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
80 °C

実験手順

In a 50-ml three-necked flask under an argon atmosphere, heat, at 80° C. for 2 hours, a solution of 3 g of the (2-amino-phenyl)amide of 9-oxo-9H-fluorene-4-carboxylic acid obtained in the preceding stage, in 150 ml of acetic acid. After cooling, the precipitate that formed is drained. After purification by silica gel flash chromatography, eluting with mixtures of dichloromethane and ethyl acetate (90-10 then 80-20 and finally 70-30 by volume), we obtain 1.73 g of 4-(1H-benzimidazol-2-yl)-fluoren-9-one in the form of a yellow powder, which is used as it is in the next stage, with the following characteristics:

後処理

  1. temperatureAfter cooling
  2. customthe precipitate that formed
  3. customAfter purification by silica gel flash chromatography
  4. washeluting with mixtures of dichloromethane and ethyl acetate (90-10

出典と根拠

ORDレコード
ord-91000b449a9f4adba18f981a768e6866
出典データセット
uspto-grants-2010_03
特許番号
US07674795B2

関連ノート

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