Nitric Acid → HCID 67280656, 화합물

HRID 1693335노트

반응식

HRID 1693335 반응식
[Cl:1][C:2]1[C:3]([CH3:10])=[N+:4]([O-:9])[CH:5]=[C:6]([CH3:8])[CH:7]=1.[N+:11]([O-])([OH:13])=[O:12].C(=O)([O-])[O-].[NH4+].[NH4+]>S(=O)(=O)(O)O>[Cl:1][C:2]1[C:3]([CH3:10])=[N+:4]([O-:9])[CH:5]=[C:6]([CH3:8])[C:7]=1[N+:11]([O-:13])=[O:12]

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 517111Ammonium CarbonateHCID 67279710Pyridine, 3-chloro-2,5-dimethyl-, 1-oxide

생성물 1

HCID 67280656HCID 67280656, 화합물수율 72%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

실험 절차

The above 3-chloro-2,5-dimethylpyridine 1-oxide (1.20 g) was dissolved in concentrated sulfuric acid (6 mL), and a mixture of fuming nitric acid (9.5 mL) and fuming sulfuric acid (5.5 mL) was added dropwise over 25 minutes. After stirring in that state for 30 minutes, the mixture was stirred at 90° C. for two hours. The reaction solution was left to cool, and then introduced into ice water and neutralized with ammonium carbonate with stirring at room temperature. The insoluble matter was separated off by filtration, followed by extraction with chloroform. The organic layer was dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (chloroform-methanol) to obtain the title compound (1.11 g, 72%) as a solid.

후처리

  1. additionwas added dropwise over 25 minutes
  2. stirringthe mixture was stirred at 90° C. for two hours
  3. waitThe reaction solution was left
  4. temperatureto cool
  5. stirringwith stirring at room temperature
  6. customThe insoluble matter was separated off by filtration
  7. extractionfollowed by extraction with chloroform
  8. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  9. customThe solvent was evaporated under reduced pressure
  10. customthe residue was purified by silica gel column chromatography (chloroform-methanol)

출처 및 근거

ORD 기록
ord-e89e2b43688d44008dc6b8f190574a68
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08158638B2

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