O-Phenylenediamine → 2-(4-Hydroxy-3-methoxy-5-nitrophenyl)quinoxaline

HRID 274465

반응식

HRID 274465 반응식
Br[CH2:2][C:3]([C:5]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[C:8]([OH:14])=[C:7]([O:15][CH3:16])[CH:6]=1)=O.[C:17]1([NH2:24])[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[NH2:23].C([O-])(=O)C.[Na+]>CO>[OH:14][C:8]1[C:9]([N+:11]([O-:13])=[O:12])=[CH:10][C:5]([C:3]2[CH:2]=[N:24][C:17]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[N:23]=2)=[CH:6][C:7]=1[O:15][CH3:16]

참가 물질

5

반응물 3

HCID 7243O-PhenylenediamineHCID 517045Sodium AcetateHCID 144509832-Bromo-4'-hydroxy-3'-methoxy-5'-nitroacetophenone

생성물 1

HCID 1356653242-(4-Hydroxy-3-methoxy-5-nitrophenyl)quinoxaline

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

ada) A suspension of 14.5 g of 2-bromo-4'-hydroxy-3'-methoxy-5'-nitroacetophenone and 5.41 g of 1,2-phenylenediamine in 350 ml of methanol is treated with 4.92 g of sodium acetate and the mixture is heated to boiling under reflux for 22 hours. The reaction mixture is then evaporated, the residue is dissolved in methylene chloride, this solution is washed four times with water, dried over sodium sulfate, filtered and evaporated. There is obtained 2-(4-hydroxy-3-methoxy-5-nitrophenyl)quinoxaline of m.p. 195°-197° (from methylene chloride/methanol).

후처리

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 22 hours
  3. customThe reaction mixture is then evaporated
  4. dissolutionthe residue is dissolved in methylene chloride
  5. washthis solution is washed four times with water
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. customevaporated

출처 및 근거

ORD 기록
ord-e6c00635e9fa49eabf0aeab3dc375b79
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05389653

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