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

HRID 1640953

반응식

HRID 1640953 반응식
[N+:1]1([O-:9])[C:2]([CH3:8])=[CH:3][CH:4]=[CH:5][C:6]=1[CH3:7].[N+:10]([O-])([OH:12])=[O:11]>S(=O)(=O)(O)O>[N+:10]([C:4]1[CH:3]=[C:2]([CH3:8])[N+:1]([O-:9])=[C:6]([CH3:7])[CH:5]=1)([O-:12])=[O:11]

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 140832,6-Dimethylpyridine N-oxide

생성물 1

HCID 209452,6-Lutidine, 4-nitro-, 1-oxide

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

A mixture of 2,6-lutidine 1-oxide (20, 15 g, 110 mmol) and concentrated sulfuric acid (98%, 30 ml) and concentrated nitric acid (70%, 12 ml) is heated under reflux for 3 hours. The mixture is poured into a large excess of ice and extracted with chloroform (3×100 ml). The combined chloroform extracts are washed with aqueous sodium hydroxide and water and dried over magnesium sulfate. Removal of the solvent yields pure yellow solid 4-Nitro-2,6-lutidine 1-oxide (21). 1H NMR (300 MHz, CDCl3) δ 2.64 (s, 6H), 8.08 (s, 2H). MS, m/z 169 (M+1), 210 (M+MeCN).

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 3 hours
  3. additionThe mixture is poured into a large excess of ice
  4. extractionextracted with chloroform (3×100 ml)
  5. washThe combined chloroform extracts are washed with aqueous sodium hydroxide and water
  6. dry with materialdried over magnesium sulfate
  7. customRemoval of the solvent

출처 및 근거

ORD 기록
ord-7093bf396e344b2baa5da26007741495
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08114888B2

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