9-Oxofluorene-4-carboxylic acid → HCID 67359009、化合物

HRID 2243324

反応式

HRID 2243324 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[NH-:9].[O:10]=[C:11]1[C:23]2[CH:22]=[CH:21][CH:20]=[C:19]([C:24](O)=O)[C:18]=2[C:17]2[C:12]1=[CH:13][CH:14]=[CH:15][CH:16]=2.C(=O)([O-])O.[Na+]>C(O)(=O)C.O>[CH3:8][C:4]1[C:3]2[N:9]=[C:24]([C:19]3[C:18]4[C:17]5[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=5)[C:11](=[O:10])[C:23]=4[CH:22]=[CH:21][CH:20]=3)[NH:1][C:2]=2[CH:7]=[CH:6][CH:5]=1

参加物

6

反応物 3

HCID 803619-Oxofluorene-4-carboxylic acidHCID 516892Sodium BicarbonateHCID 86621029HCID 86621029、化合物

生成物 1

HCID 67359009HCID 67359009、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

The procedure used in Example 68 is followed. In a 250 ml round-bottomed flask under an argon atmosphere, reflux, for 6 hours, a suspension of 5 g of (2-amino-6-methylphenyl)amide of 9-oxo-9H-fluorene-4-carboxylic acid, obtained in the previous stage, in 100 ml of acetic acid. After cooling, bring to dryness under reduced pressure. Take the residue up in 25 ml of water then bring to pH=8 by addition of a saturated aqueous solution of sodium hydrogen carbonate. The precipitate that formed is filtered off, washed with water, and made into a paste with diisopropyl ether, and in this way, we obtain 4.7 g of 4-(4-methyl-1H-benzimidazol-2-yl)-9H-fluoren-9-one, in the form of an orange powder, which is used as it is in the following stage, with the following characteristics:

後処理

  1. temperatureIn a 250 ml round-bottomed flask under an argon atmosphere, reflux, for 6 hours
  2. temperatureAfter cooling
  3. customThe precipitate that formed
  4. filtrationis filtered off
  5. washwashed with water

出典と根拠

ORDレコード
ord-dddcc537beb54a5384c268608f75438e
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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