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

HRID 2071155

반응식

HRID 2071155 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 209452,6-Lutidine, 4-nitro-, 1-oxide수율 76%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7294282d81874981a4d8835a09f100bd
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08299267B2

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