Benzenamine, 4-chloro-2-methoxy- → 4-Chloro-2-methoxy-5-nitroaniline

HRID 1512990노트

반응식

HRID 1512990 반응식
[Cl:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([O:9][CH3:10])[CH:3]=1.[N+:11]([O-])([OH:13])=[O:12].NC(N)=N.C(=O)([O-])[O-].[Na+].[Na+]>S(=O)(=O)(O)O>[Cl:1][C:2]1[C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:5]([NH2:6])=[C:4]([O:9][CH3:10])[CH:3]=1

참가 물질

5

반응물 3

HCID 7143Benzenamine, 4-chloro-2-methoxy-HCID 10340Sodium CarbonateHCID 10481Guanidine Nitrate

생성물 1

HCID 593100544-Chloro-2-methoxy-5-nitroaniline수율 80.3%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

To a suspension of 4-chloro-2-methoxyaniline (1.88 g) in concentrated sulfuric acid (18 mL) was added guanidine nitrate (1.46 g) under ice-cooling over 15 minutes, and the mixture was stirred at the same temperature for 15 minutes. The reaction mixture was poured into a saturated aqueous sodium carbonate solution cooled in ice, and the precipitated crystals were collected by filtration. The crystals were dissolved in ethyl acetate, and the solution was dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure to give the title compound (1.94 g).

후처리

  1. temperaturecooling over 15 minutes
  2. temperaturecooled in ice
  3. filtrationthe precipitated crystals were collected by filtration
  4. dissolutionThe crystals were dissolved in ethyl acetate
  5. dry with materialthe solution was dried over anhydrous magnesium sulfate
  6. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-d7e4eb6ebd8a4b7ea8de81c5d6993397
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217069B2

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