Methyl iodide → 4-Methoxy-N-methyl-2-nitrobenzenamine

HRID 230000

反応式

HRID 230000 の反応式
[CH3:1][O:2][C:3]1[CH:9]=[CH:8][C:6]([NH2:7])=[C:5]([N+:10]([O-:12])=[O:11])[CH:4]=1.[H-].[Na+].CI.[C:17]([O-])(O)=O.[Na+]>CN(C=O)C.[Cl-].[Na+].O>[CH3:17][NH:7][C:6]1[CH:8]=[CH:9][C:3]([O:2][CH3:1])=[CH:4][C:5]=1[N+:10]([O-:12])=[O:11]

参加物

7

反応物 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 667934-Methoxy-2-nitroanilineHCID 516892Sodium Bicarbonate

生成物 1

HCID 35543134-Methoxy-N-methyl-2-nitrobenzenamine

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

To 4-methoxy-2-nitroaniline (10 mmol, 1.68 g) in 20 mL of DMF was added NaH (12 mmol, 480 mg of a 60% dispersion in mineral oil) (exothermic, H2 evolution), affording a deep red slurry. After 15 min MeI (20 mmol, 1.2 mL) was added (exothermic). After 30 min the reaction was poured into a solution of brine and NaHCO3, resulting in formation of a bright orange precipitate. The slurry was filtered and the filter cake was washed with H2O. The solid was dried under reduced pressure, affording a bright orange solid. HPLC A: 1.77 min.

後処理

  1. customaffording a deep red slurry
  2. customresulting in formation of a bright orange precipitate
  3. filtrationThe slurry was filtered
  4. washthe filter cake was washed with H2O
  5. customThe solid was dried under reduced pressure
  6. customaffording a bright orange solid
  7. custom1.77 min.

出典と根拠

ORDレコード
ord-0681ef451e024f8f8ef93e82d1e8a705
出典データセット
uspto-grants-2009_07
特許番号
US07563815B2

関連ノート

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