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Ammonium Chloride → HCID 13750559、化合物

HRID 1593388
ノート
印刷プレビュー

反応式

HRID 1593388 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[N:11][C:10]2[C:5](=[CH:6][CH:7]=[C:8]([N+:13]([O-])=O)[CH:9]=2)[N:4]=1.[Cl-].[NH4+]>[Fe].CO>[CH3:1][O:2][C:3]1[CH:12]=[N:11][C:10]2[C:5](=[CH:6][CH:7]=[C:8]([NH2:13])[CH:9]=2)[N:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 25517Ammonium ChlorideHCID 150258562-Methoxy-6-nitroquinoxaline

生成物 1

HCID 13750559HCID 13750559、化合物収率 124.2%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 887Methanol溶媒

実験手順

Into 20 ml of methanol was dissolved 726 mg of 2-methoxy-6-nitroquinoxaline, and then 1.0 g of iron powder and a saturated ammonium chloride aqueous solution were added thereto, followed by heating under refluxing overnight. Insoluble matter was separated by filtration using celite and then the solvent was removed by evaporation. A sodium bicarbonate aqueous solution was added to the residue, followed by extraction with ethyl acetate. After the organic layer was dried over anhydrous magnesium sulfate, the solvent was removed by evaporation and the resulting residue was purified by silica gel column chromatography to obtain 770 mg of the title compound from chloroform-methanol (100:1, v/v).

後処理

  1. temperatureby heating
  2. temperatureunder refluxing overnight
  3. customInsoluble matter was separated by filtration
  4. customthe solvent was removed by evaporation
  5. additionA sodium bicarbonate aqueous solution was added to the residue
  6. extractionfollowed by extraction with ethyl acetate
  7. dry with materialAfter the organic layer was dried over anhydrous magnesium sulfate
  8. customthe solvent was removed by evaporation
  9. customthe resulting residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-85072f7ac6b0466e97421e2f1f72ce56
出典データセット
uspto-grants-2007_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07297698B2

反応ノート

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