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Chlorine monoxide → 6-chloro-3-methyl-7H-indeno[2,1-c]quinoline-7-on

HRID 726681
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HRID 726681 반응식
[CH3:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]3[C:19]4[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=4)[C:13](=[O:20])[C:7]=3[C:8](=O)[NH:9]2)=[CH:4][CH:3]=1.O(Cl)[Cl:22]>>[Cl:22][C:8]1[C:7]2[C:13](=[O:20])[C:14]3[C:19]([C:6]=2[C:5]2[C:10](=[CH:11][C:2]([CH3:1])=[CH:3][CH:4]=2)[N:9]=1)=[CH:18][CH:17]=[CH:16][CH:15]=3
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 24646Chlorine monoxideHCID 19356120HCID 19356120, 화합물

생성물 1

HCID 193561186-chloro-3-methyl-7H-indeno[2,1-c]quinoline-7-on수율 73.4%

실험 절차

A mixture of 3-methyl-5H-indeno[2,1-c]quinoline-6,7-dion obtained in reference example 5 (700 mg, 2.7 mmol) and phophorous oxychloride (10 ml, 107 mmol) was refluxed with heat for 1.5 hours. The reaction mixture was distilled to dryness. To the residue was added water to obtain a crystal precipitated by filtration. The crystal obtained was washed with water and dissolved in chloroform to filter off undissolved substances. Recrystallization from benzene to give 550 mg (yield 73.4%) of the title compound.

후처리

  1. temperaturewas refluxed
  2. temperaturewith heat for 1.5 hours
  3. distillationThe reaction mixture was distilled to dryness
addition
To the residue was added water
  • customto obtain a crystal
  • customprecipitated by filtration
  • customThe crystal obtained
  • washwas washed with water
  • dissolutiondissolved in chloroform
  • filtrationto filter off undissolved substances
  • customRecrystallization from benzene
  • 출처 및 근거

    ORD 기록
    ord-1e0a2fba45c5448b951eb1d8531b297f
    출처 데이터셋
    uspto-grants-1998_01
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05710162

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