Pyridine → N-(3-(pyrazin-2-yl)phenyl)-9H-fluorene-1-carboxamide

HRID 1835443ノート

反応式

HRID 1835443 の反応式
[N:1]1[CH:6]=[CH:5][N:4]=[CH:3][C:2]=1[C:7]1[CH:8]=[C:9]([CH:11]=[CH:12][CH:13]=1)[NH2:10].N1C=CC=CC=1.[C:20]1([C:33](Cl)=[O:34])[C:32]2[CH2:31][C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[C:24]=2[CH:23]=[CH:22][CH:21]=1>ClCCl>[N:1]1[CH:6]=[CH:5][N:4]=[CH:3][C:2]=1[C:7]1[CH:8]=[C:9]([NH:10][C:33]([C:20]2[C:32]3[CH2:31][C:30]4[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=4)[C:24]=3[CH:23]=[CH:22][CH:21]=2)=[O:34])[CH:11]=[CH:12][CH:13]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 255028Fluorene-1-carbonyl chlorideHCID 235036723-(Pyrazin-2-yl)aniline

生成物 1

HCID 23503682N-(3-(pyrazin-2-yl)phenyl)-9H-fluorene-1-carboxamide収率 76%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

To a suspension of 3-(pyrazin-2-yl)aniline (0.12g) and pyridine (0.17ml) in dichloromethane (3ml) was dropwise added a solution of the fluorene-1-carbonyl chloride (0.16 g) in dichloromethane (3 ml) followed by stirring for 2 hours. The mixture was diluted with dichloromethane and washed with an aqueous solution of sodium hydrogen carbonate and brine. The separated organic layer was dried over sodium sulfate and evaporated under reduced pressure. The residue was purified by a silica gel column chromatography eluting with 2% methanol in dichloromethane to give N-(3-(pyrazin-2-yl)phenyl)-9H-fluorene-1-carboxamide (0.193 g; 76.0%).

後処理

  1. washwashed with an aqueous solution of sodium hydrogen carbonate and brine
  2. dry with materialThe separated organic layer was dried over sodium sulfate
  3. customevaporated under reduced pressure
  4. customThe residue was purified by a silica gel column chromatography
  5. washeluting with 2% methanol in dichloromethane

出典と根拠

ORDレコード
ord-2158a663affa414a94039e6fe35970a5
出典データセット
uspto-grants-2004_08
特許番号
US06770667B1

反応ノート

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