Nitric Acid → Pyridine, 2-methyl-4-nitro-, 1-oxide

HRID 963475

反応式

HRID 963475 の反応式
S(=O)(=O)(O)O.[N+:6]1([O-:13])[C:7]([CH3:12])=[CH:8][CH:9]=[CH:10][CH:11]=1.[N+:14]([O-])([OH:16])=[O:15].[OH-].[Na+]>O>[N+:14]([C:9]1[CH:8]=[C:7]([CH3:12])[N+:6]([O-:13])=[CH:11][CH:10]=1)([O-:16])=[O:15]

参加物

6

反応物 4

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 136022-Methylpyridine 1-oxideHCID 14798Sodium Hydroxide

生成物 1

HCID 95291Pyridine, 2-methyl-4-nitro-, 1-oxide

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

98% sulfuric acid (17.5 ml) was added dropwise to 2-picoline-1-oxide (5.22 g) under stirring at cooling in an ice-bath. To the mixture was added dropwise nitric acid (fuming, 15 ml) under the same condition. After completion of the additieon, the mixture was heated at 80°-90° C. for 2 hours. The reaction mixture was allowed to cool to room temperature, poured into water (100 ml) and alkalined with aN aqueous sodium hydroxide. The resultant mixture was extracted with chloroform four times. The combined extracts were dried over sodium sulfate. Removal of the solvent gave 4-nitro-2-picoline-1-oxide (6.52 g).

後処理

  1. temperatureat cooling in an ice-bath
  2. temperatureAfter completion of the additieon, the mixture was heated at 80°-90° C. for 2 hours
  3. extractionThe resultant mixture was extracted with chloroform four times
  4. dry with materialThe combined extracts were dried over sodium sulfate
  5. customRemoval of the solvent

出典と根拠

ORDレコード
ord-074ed863a1614baca9f8a10afa12ac57
出典データセット
uspto-grants-1998_06
特許番号
US05763437

関連ノート

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