Nitric Acid → 2,3-Dimethyl-4-nitropyridine-N-oxide

HRID 35454

反応式

HRID 35454 の反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][N+:3]=1[O-:9].[N+:10]([O-])([OH:12])=[O:11].C(=O)([O-])[O-].[Na+].[Na+]>S(=O)(=O)(O)O>[CH3:1][C:2]1[C:7]([CH3:8])=[C:6]([N+:10]([O-:12])=[O:11])[CH:5]=[CH:4][N+:3]=1[O-:9]

参加物

5

反応物 3

HCID 944Nitric AcidHCID 10340Sodium CarbonateHCID 3840573Pyridine, 2,3-dimethyl-, 1-oxide

生成物 1

HCID 1482232,3-Dimethyl-4-nitropyridine-N-oxide

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

A solution of 183 mg (1.49 mmol) of 2,3-dimethylpyridine 1-oxide in 0.6 ml of conc. sulphuric acid is treated while coollng with ice with 0.2 ml of 65% nitric acid (d=1.4). The reaction mixture is stirred at 9° for 24 hours and poured on to a mixture of ice and sodium carbonate, whereupon the resulting mixture is extracted with methylene chloride and the methylene chloride phase is dried and evaporated. The residue crystallized from ethanol/n-pentane, gives 2,3-dimethyl-4-nitropyridine 1-oxide of melting point 99°-102°.

後処理

  1. extractionis extracted with methylene chloride
  2. dry with materialthe methylene chloride phase is dried
  3. customevaporated
  4. customThe residue crystallized from ethanol/n-pentane

出典と根拠

ORDレコード
ord-2bf7fb5403744011940384733b58d710
出典データセット
uspto-grants-1988_08
特許番号
US04766133

関連ノート

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