Nitric Acid → 2,6-Lutidine, 4-nitro-, 1-oxide

HRID 2071155

反応式

HRID 2071155 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[N+:3]=1[O-:9].C(Cl)(Cl)Cl.O.[N+:15]([O-])([OH:17])=[O:16]>OS(O)(=O)=O>[CH3:1][C:2]1[CH:7]=[C:6]([N+:15]([O-:17])=[O:16])[CH:5]=[C:4]([CH3:8])[N+:3]=1[O-:9]

参加物

6

反応物 4

HCID 944Nitric AcidHCID 962WaterHCID 6212ChloroformHCID 140832,6-Dimethylpyridine N-oxide

生成物 1

HCID 209452,6-Lutidine, 4-nitro-, 1-oxide収率 76%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

A solution of 2.23 g (18.1 mmol) of 2,6-dimethylpyridine 1-oxide (Alfa Aesar) in 7 mL of H2SO4 and 2.7 mL of HNO3 was stirred at 130° C. for 23.5 h. The solution was added to ice with CHCl3 and H2O, and the aqueous layer was extracted with CHCl3 (2×). The combined extracts were washed with 75 mL of saturated NaHCO3 solution, and the aqueous layer was extracted with CHCl3. The combined extracts were washed with brine, dried over Na2SO4, filtered, and concentrated to give 2.3 g of 2,6-dimethyl-4-nitropyridine 1-oxide in 76% yield which was used without further purification.

後処理

  1. extractionthe aqueous layer was extracted with CHCl3 (2×)
  2. washThe combined extracts were washed with 75 mL of saturated NaHCO3 solution
  3. extractionthe aqueous layer was extracted with CHCl3
  4. washThe combined extracts were washed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-7294282d81874981a4d8835a09f100bd
出典データセット
uspto-grants-2012_10
特許番号
US08299267B2

関連ノート

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