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

HRID 963475

반응식

HRID 963475 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-074ed863a1614baca9f8a10afa12ac57
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05763437

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