Hydrochloric Acid → 4-Methoxy-2,3,5-trimethylpyridine 1-oxide

HRID 35469

反応式

HRID 35469 の反応式
[Na].[CH3:2][C:3]1[C:8]([CH3:9])=[C:7]([N+]([O-])=O)[C:6]([CH3:13])=[CH:5][N+:4]=1[O-:14].Cl.[CH3:16][OH:17]>C(OCC)(=O)C>[CH3:16][O:17][C:7]1[C:6]([CH3:13])=[CH:5][N+:4]([O-:14])=[C:3]([CH3:2])[C:8]=1[CH3:9]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 5360545SodiumHCID 112176114-Nitro-2,3,5-trimethylpyridine, 1-oxide

生成物 1

HCID 107022374-Methoxy-2,3,5-trimethylpyridine 1-oxide

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

22.6 g of sodium are dissolved in 4 1 of methanol under argon. 120 g of 2,3,5-trimethyl-4-nitropyridine 1-oxide are then added portionwise thereto and the solution is left to boil under reflux overnight. The pH is adjusted to 7 by means of 5N hydrogen chloride in ethyl acetate while cooling and the mixture is then evaporated in vacuo. The residue is taken up in 1.5 1 of methylene chloride, the solution is filtered throuqh siliceous earth, which is rinsed with 0.5 1 of methylene chloride, the combined filtrates are evaporated in vacuo and the residue is crystallized from petroleum ether. There is obtained 4-methoxy-2,3,5-trimethylpyridine 1-oxide of melting point 48°-50°.

後処理

  1. waitthe solution is left
  2. temperatureunder reflux overnight
  3. temperaturewhile cooling
  4. customthe mixture is then evaporated in vacuo
  5. filtrationthe solution is filtered throuqh siliceous earth, which
  6. washis rinsed with 0.5 1 of methylene chloride
  7. customthe combined filtrates are evaporated in vacuo
  8. customthe residue is crystallized from petroleum ether

出典と根拠

ORDレコード
ord-518b8ecebb294c6991c42d564bd64b1a
出典データセット
uspto-grants-1988_08
特許番号
US04766133

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