Ammonium Chloride → 2-Methoxy-4-methyl-5-nitropyridine

HRID 1398774

反応式

HRID 1398774 の反応式
Cl[C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][N:3]=1.[CH3:12][O-:13].[Na+].[Cl-].[NH4+]>CO>[CH3:12][O:13][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][N:3]=1

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 3453642-Chloro-4-methyl-5-nitropyridineHCID 10942334Sodium Methoxide

生成物 1

HCID 2431692-Methoxy-4-methyl-5-nitropyridine収率 98%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 2-chloro-4-methyl-5-nitropyridine (3.0 g, 17.3 mmol) in methanol (20 mL) was added a solution of sodium methoxide (28% in methanol, 10 mL) dropwise at 0° C. The mixture was warmed to room temperature and stirred for 16 hr. The mixture was neutralized by addition of aqueous ammonium chloride and concentrated in vacuo. The residue was dissolved in water and extracted with ethyl acetate. Organic layer was washed with brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to give the title compound (2.84 g, 16.8 mmol, 98%) as a yellow solid.

後処理

  1. concentrationconcentrated in vacuo
  2. dissolutionThe residue was dissolved in water
  3. extractionextracted with ethyl acetate
  4. washOrganic layer was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-5af145c853f74bec9de396d8d7a0df88
出典データセット
uspto-grants-2014_12
特許番号
US08901141B2

関連ノート

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