Sulfuric Acid → 2,3,5-Trimethylpyridine

HRID 2231949ノート

反応式

HRID 2231949 の反応式
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

参加物

5

反応物 2

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

生成物 1

HCID 127592,3,5-Trimethylpyridine

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-34cdf6932df9494598878de3cecc58af
出典データセット
uspto-grants-1988_11
特許番号
US04785113

反応ノート

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