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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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6-Methoxy-2-(4-methoxyphenyl)benzo[b]thiophene → (6-Chloro-pyridin-3-yl)-[6-methoxy-2-(4-methoxy-phenyl)-benzo[b]thiophen-3-yl]-methanone

HRID 354069
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HRID 354069 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](Cl)=[O:9])=[CH:4][N:3]=1.[CH3:11][O:12][C:13]1[CH:14]=[CH:15][C:16]2[CH:20]=[C:19]([C:21]3[CH:26]=[CH:25][C:24]([O:27][CH3:28])=[CH:23][CH:22]=3)[S:18][C:17]=2[CH:29]=1.[Cl-].[Cl-].[Cl-].[Al+3]>C(Cl)Cl>[Cl:1][C:2]1[N:3]=[CH:4][C:5]([C:8]([C:20]2[C:16]3[CH:15]=[CH:14][C:13]([O:12][CH3:11])=[CH:29][C:17]=3[S:18][C:19]=2[C:21]2[CH:26]=[CH:25][C:24]([O:27][CH3:28])=[CH:23][CH:22]=2)=[O:9])=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8509416-Methoxy-2-(4-methoxyphenyl)benzo[b]thiopheneHCID 27821656-Chloronicotinoyl ChlorideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 23512898(6-Chloro-pyridin-3-yl)-[6-methoxy-2-(4-methoxy-phenyl)-benzo[b]thiophen-3-yl]-methanone수율 32.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a suspension of 2-Chloropyridine-5-carbonyl chloride (4.23 gm, 24 mmol) and 6-Methoxy-2-(4-methoxy-phenyl) -benzo[b]thiophene (5.0 gm, 18.5 mmol) in 275 mL of methylene chloride was added aluminum trichloride (18.59 g, 138.8 mmol) in three portions. The black-red reaction was stirred for 16 hrs. at room temperature. The reaction was then quenched with 400 mL of 2N NaOH (slowly and cooled in ice) and extracted into 300 mL of methylene chloride. The organic layer was washed with brine, dried over anhydrous sodium sulfate, filtered, and concentrated to a yellow solid which was chromatographed on silica gel using 5% to 20% Ethyl acetate/Hexanes as the gradient eluant to yield 2.47 gm of the title compound.

후처리

  1. customThe black-red reaction
  2. customat room temperature
  3. customThe reaction was then quenched with 400 mL of 2N NaOH (slowly and
  4. temperaturecooled in ice) and
  5. extractionextracted into 300 mL of methylene chloride
  6. washThe organic layer was washed with brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated to a yellow solid which
  10. customwas chromatographed on silica gel using 5% to 20% Ethyl acetate/Hexanes as the gradient eluant

출처 및 근거

ORD 기록
ord-7931cbc65c364b249cb01a240934fdec
출처 데이터셋
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06756388B1

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