2,3-Dimethyl-4-nitropyridine-N-oxide → Pyridine, 4-methoxy-2,3-dimethyl-, 1-oxide

HRID 35465

反応式

HRID 35465 の反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[C:6]([N+]([O-])=O)[CH:5]=[CH:4][N+:3]=1[O-:12].[CH3:13][O-:14].[Na+]>CO>[CH3:13][O:14][C:6]1[CH:5]=[CH:4][N+:3]([O-:12])=[C:2]([CH3:1])[C:7]=1[CH3:8]

参加物

4

反応物 2

HCID 1482232,3-Dimethyl-4-nitropyridine-N-oxideHCID 10942334Sodium Methoxide

生成物 1

HCID 10630707Pyridine, 4-methoxy-2,3-dimethyl-, 1-oxide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 2.5 g (0.015 mol) of 2,3-dimethyl-4-nitropyridine 1-oxide in 50 ml of abs. methanol is treated with 0.883 g of sodium methylate, whereupon the mixture is stirred at room temperature under argon for 2 days. The reaction mixture is concentrated and the residue is extracted with methylene chloride and saturated sodium chloride solution. The methylene chloride phase is dried and evaporated. The residue, crystallized from methylene chloride/ ether, gives 4-methoxy-2,3-dimethylpyridine 1-oxide of melting point 80°-83°.

後処理

  1. concentrationThe reaction mixture is concentrated
  2. extractionthe residue is extracted with methylene chloride and saturated sodium chloride solution
  3. dry with materialThe methylene chloride phase is dried
  4. customevaporated
  5. customThe residue, crystallized from methylene chloride/ ether

出典と根拠

ORDレコード
ord-3bf28547df6047c298170f041a6da9a4
出典データセット
uspto-grants-1988_08
特許番号
US04766133

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