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

HRID 1512990ノート

反応式

HRID 1512990 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 593100544-Chloro-2-methoxy-5-nitroaniline収率 80.3%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d7e4eb6ebd8a4b7ea8de81c5d6993397
出典データセット
uspto-grants-2012_07
特許番号
US08217069B2

反応ノート

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