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Ammonium Chloride → HCID 13750559, 화합물

HRID 1593388
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HRID 1593388 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 25517Ammonium ChlorideHCID 150258562-Methoxy-6-nitroquinoxaline

생성물 1

HCID 13750559HCID 13750559, 화합물수율 124.2%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-85072f7ac6b0466e97421e2f1f72ce56
출처 데이터셋
uspto-grants-2007_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07297698B2

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