9-Oxofluorene-4-carboxylic acid → HCID 59208194, 화합물

HRID 2243314

반응식

HRID 2243314 반응식
[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

참가 물질

4

반응물 2

HCID 803619-Oxofluorene-4-carboxylic acidHCID 86621027HCID 86621027, 화합물

생성물 1

HCID 59208194HCID 59208194, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
80 °C

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-91000b449a9f4adba18f981a768e6866
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07674795B2

연결된 노트

불러오는 중…