Water → 2-Methoxy-4-methyl-5-nitropyridine

HRID 53528

反応式

HRID 53528 の反応式
[CH3:1][O-:2].[Na+].Cl[C:5]1[CH:10]=[C:9]([CH3:11])[C:8]([N+:12]([O-:14])=[O:13])=[CH:7][N:6]=1.O>CO>[CH3:1][O:2][C:5]1[CH:10]=[C:9]([CH3:11])[C:8]([N+:12]([O-:14])=[O:13])=[CH:7][N:6]=1

参加物

5

反応物 3

HCID 962WaterHCID 3453642-Chloro-4-methyl-5-nitropyridineHCID 10942334Sodium Methoxide

生成物 1

HCID 2431692-Methoxy-4-methyl-5-nitropyridine収率 55.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Sodium methoxide (26.1 g) was added to a solution of 2-chloro-4-methyl-5-nitropyridine (19.0 g) in methanol (100 ml) and the resulting mixture was refluxed for 12 hours. Upon cooling, the mixture was poured over water (1 L), and the product was extracted with ethyl acetate and washed with water. The organic phase was dried (anhydrous magnesium sulfate) and concentrated, and the residue dissolved in hot ether and filtered. Crystallization from ether provided 10.2 g of the title compound, suitable for use in the next reaction.

後処理

  1. temperaturethe resulting mixture was refluxed for 12 hours
  2. temperatureUpon cooling
  3. extractionthe product was extracted with ethyl acetate
  4. washwashed with water
  5. dry with materialThe organic phase was dried (anhydrous magnesium sulfate)
  6. concentrationconcentrated
  7. dissolutionthe residue dissolved in hot ether
  8. filtrationfiltered
  9. customCrystallization from ether

出典と根拠

ORDレコード
ord-3d639581d26c44ddb7f10dbba34ccf92
出典データセット
uspto-grants-1997_04
特許番号
US05620974

関連ノート

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