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

HRID 1835443노트

반응식

HRID 1835443 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-2158a663affa414a94039e6fe35970a5
출처 데이터셋
uspto-grants-2004_08
특허 번호
US06770667B1

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