9-Oxofluorene-4-carboxylic acid → HCID 67359009, 화합물

HRID 2243324

반응식

HRID 2243324 반응식
[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

참가 물질

6

반응물 3

HCID 803619-Oxofluorene-4-carboxylic acidHCID 516892Sodium BicarbonateHCID 86621029HCID 86621029, 화합물

생성물 1

HCID 67359009HCID 67359009, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-dddcc537beb54a5384c268608f75438e
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07674795B2

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