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Pyridine → N-(4-methyl-3-(pyrimidin-5-yl)-phenyl)-9H-fluorene-1-carboxamide

HRID 1835467
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HRID 1835467 반응식
[CH3:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][C:3]=1[C:9]1[CH:10]=[N:11][CH:12]=[N:13][CH:14]=1.N1C=CC=CC=1.[C:21]1([C:34](Cl)=[O:35])[C:33]2[CH2:32][C:31]3[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=3)[C:25]=2[CH:24]=[CH:23][CH:22]=1>ClCCl>[CH3:1][C:2]1[CH:8]=[CH:7][C:5]([NH:6][C:34]([C:21]2[C:33]3[CH2:32][C:31]4[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=4)[C:25]=3[CH:24]=[CH:23][CH:22]=2)=[O:35])=[CH:4][C:3]=1[C:9]1[CH:14]=[N:13][CH:12]=[N:11][CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 255028Fluorene-1-carbonyl chlorideHCID 235036604-Methyl-3-(pyrimidin-5-yl)aniline

생성물 1

HCID 23503685N-(4-methyl-3-(pyrimidin-5-yl)-phenyl)-9H-fluorene-1-carboxamide수율 73.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

To a suspension of 4-methyl-3-(pyrimidin-5-yl)aniline (0.111 g) and pyridine (0.15 ml) in dichloromethane (2 ml) was dropwise added a solution of the fluorene-1-carbonyl chloride (0.137 g) in dichloromethane (2 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 triturated with methanol. The resulting solid was collected by filtration to give N-(4-methyl-3-(pyrimidin-5-yl)-phenyl)-9H-fluorene-1-carboxamide (0.167 g, 73.9%)

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 triturated with methanol
  5. filtrationThe resulting solid was collected by filtration

출처 및 근거

ORD 기록
ord-9e4636e5e4334990a367db70e3b23575
출처 데이터셋
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06770667B1

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