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Dimethylformamide → N6-Methoxy-7-benzyloxy-4-chloro-6-quinolinecarboxamide

HRID 388077
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HRID 388077 반응식
S(Cl)(Cl)=O.CN(C)C=O.[CH2:10]([O:17][C:18]1[CH:27]=[C:26]2[C:21]([C:22](=O)[CH:23]=[CH:24][NH:25]2)=[CH:20][C:19]=1[C:29]([O:31]C1C=CC=CC=1)=O)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[ClH:38].[O:39]([NH2:41])[CH3:40]>C(OCC)(=O)C.CCCCCC.O>[CH3:40][O:39][NH:41][C:29]([C:19]1[CH:20]=[C:21]2[C:26](=[CH:27][C:18]=1[O:17][CH2:10][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1)[N:25]=[CH:24][CH:23]=[C:22]2[Cl:38])=[O:31]
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참가 물질

8

반응물 4

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 521874O-Methylhydroxylamine hydrochlorideHCID 22936353Phenyl 7-benzyloxy-4-oxo-1,4-dihydro-6-quinolinecarboxylate

생성물 1

HCID 22936829N6-Methoxy-7-benzyloxy-4-chloro-6-quinolinecarboxamide수율 18.2%

시약·촉매·용매 3

HCID 962
Water
용매
HCID 8058Hexane용매
HCID 8857Ethyl Acetate용매2회

실험 절차

After adding thionyl chloride (10 ml) and a catalytic amount of dimethylformamide to phenyl 7-benzyloxy-4-oxo-1,4-dihydro-6-quinolinecarboxylate (2.32 g, 6.25 mmol), the mixture was heated to reflux for 2 hours while stirring. The reaction solution was concentrated under reduced pressure and azeotropically distilled twice with toluene, the residue was dissolved in a dimethylformamide (20 ml) and triethylamine (20 ml) mixed solvent, methoxylamine hydrochloride (10.4 g, 125 mmol) was added thereto while cooling in an ice water bath, and the mixture was stirred at room temperature for 18 hours. The reaction solution was distributed between ethyl acetate and water, and then the organic layer was washed with water and saturated saline and dried over anhydrous magnesium sulfate. After distilling off the solvent, it was subjected to silica gel column chromatography, the target fraction was concentrated under reduced pressure, the obtained crude product was suspended in ethyl acetate, the suspension was diluted with hexane, and the crystals were filtered out, washed with hexane and blow-dried to obtain the title compound (392 mg, 1.14 mmol, 18%) as white crystals.

후처리

  1. temperatureto reflux for 2 hours
  2. concentrationThe reaction solution was concentrated under reduced pressure
  3. distillationazeotropically distilled twice with toluene
  4. dissolutionthe residue was dissolved in a dimethylformamide (20 ml) and triethylamine (20 ml)
  5. additionwas added
  6. temperaturewhile cooling in an ice water bath
  7. stirringthe mixture was stirred at room temperature for 18 hours
  8. washthe organic layer was washed with water and saturated saline
  9. dry with materialdried over anhydrous magnesium sulfate
  10. distillationAfter distilling off the solvent, it
  11. concentrationthe target fraction was concentrated under reduced pressure
  12. customthe obtained crude product
  13. filtrationthe crystals were filtered out
  14. washwashed with hexane
  15. customblow-dried

출처 및 근거

ORD 기록
ord-e286ec647987460981b1125720868f23
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08372981B2

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