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Triphosgene → HCID 22132638, 화합물

HRID 1857290
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HRID 1857290 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[CH:8][CH:7]=[C:6]2[O:15][C:16]1[CH:21]=[CH:20][C:19]([NH2:22])=[CH:18][CH:17]=1.ClC(Cl)([O:26]C(=O)OC(Cl)(Cl)Cl)Cl.[Cl:35][CH2:36][CH2:37][CH2:38][NH:39][C:40]1C=CC=CC=1.C(=O)([O-])O.[Na+]>C1(C)C=CC=CC=1.C(N(CC)CC)C>[Cl:35][CH2:36][CH2:37][CH2:38][NH:39][C:40]([NH:22][C:19]1[CH:18]=[CH:17][C:16]([O:15][C:6]2[C:5]3[C:10](=[CH:11][C:12]([O:13][CH3:14])=[C:3]([O:2][CH3:1])[CH:4]=3)[N:9]=[CH:8][CH:7]=2)=[CH:21][CH:20]=1)=[O:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 94429TriphosgeneHCID 516892Sodium BicarbonateHCID 115945434-[(6,7-Dimethoxyquinolin-4-yl)oxy]anilineHCID 18539042N-(3-Chloropropyl)aniline

생성물 1

HCID 22132638HCID 22132638, 화합물수율 37.1%

시약·촉매·용매 2

HCID 1140Toluene
용매
HCID 8471Triethylamine용매

실험 절차

6,7-Dimethoxy-4-(4-aminophenoxy)quinoline (50 mg) was dissolved in toluene (5 ml) with heat, after the addition of triethylamine (1 ml), triphosgene (55 mg) was added, and the admixture was refluxed with heat for 3 minutes. 3-Chloropropylaniline (66 mg) was added to the reaction mixture, and the admixture was refluxed with heat for 20 minutes. After the addition of aqueous sodium hydrogen carbonate, the reaction mixture was extracted 2 times with ethyl acetate, and the organic layer was then washed with brine and dried with anhydrous sodium sulfate. The solvent was removed by reduced-pressure distillation, and the resulting residue was purified by column chromatography on silica gel eluting with chloroform/acetone (10/1) to obtain 26 mg of the title compound (yield: 37%).

후처리

  1. temperaturewith heat
  2. additionwas added
  3. temperaturethe admixture was refluxed
  4. temperaturewith heat for 3 minutes
  5. temperaturethe admixture was refluxed
  6. temperaturewith heat for 20 minutes
  7. extractionthe reaction mixture was extracted 2 times with ethyl acetate
  8. washthe organic layer was then washed with brine
  9. dry with materialdried with anhydrous sodium sulfate
  10. customThe solvent was removed by reduced-pressure distillation
  11. customthe resulting residue was purified by column chromatography on silica gel eluting with chloroform/acetone (10/1)

출처 및 근거

ORD 기록
ord-af8bf5a00f0447c19eaa8c1e3153238e
출처 데이터셋
uspto-grants-2000_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06143764

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