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

HRID 1010469
ノート
印刷プレビュー

反応式

HRID 1010469 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 8058Hexane溶媒
HCID 8857Ethyl Acetate溶媒2 回

実験手順

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 brine 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.

後処理

  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 brine
  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

出典と根拠

ORDレコード
ord-502fd14fd1bc4887bc1bc0bc215653da
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07973160B2

反応ノート

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