Sulfuric Acid → 2,3,5-Trimethylpyridine

HRID 2231949노트

반응식

HRID 2231949 반응식
Cl[C:2]1[C:7]([CH3:8])=[C:6](Cl)[N:5]=[C:4]([CH3:10])[C:3]=1[CH3:11].OS(O)(=O)=O>C(O)C.[Zn]>[CH3:10][C:4]1[C:3]([CH3:11])=[CH:2][C:7]([CH3:8])=[CH:6][N:5]=1

참가 물질

5

반응물 2

HCID 1118Sulfuric AcidHCID 27791392,4-Dichloro-3,5,6-trimethylpyridine

생성물 1

HCID 127592,3,5-Trimethylpyridine

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 702Ethanol용매

실험 절차

3,8 g (20 mmoles) of 4.6-dichloro-2,3,5-trimethylpyridine are dissolved in a small amount of ethanol and treated with 5 g of zinc powder. After addition of 10 ml of 2 N H2SO4, the mixture is refluxed for 1 hour. After cooling and filtering the solution is treated with NaOH to adjust a pH of 6. The precipitated zinc salts are removed by filtration and the filtrate is extracted three times with petrol ether. After drying and evaporation 2.0 g (83%) of 2,3,5-trimethylpyridine are obtained.

후처리

  1. temperaturethe mixture is refluxed for 1 hour
  2. temperatureAfter cooling
  3. filtrationfiltering the solution
  4. additionis treated with NaOH
  5. customThe precipitated zinc salts are removed by filtration
  6. extractionthe filtrate is extracted three times with petrol ether
  7. customAfter drying
  8. customevaporation 2.0 g (83%) of 2,3,5-trimethylpyridine
  9. customare obtained

출처 및 근거

ORD 기록
ord-34cdf6932df9494598878de3cecc58af
출처 데이터셋
uspto-grants-1988_11
특허 번호
US04785113

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