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

HRID 2354058

反応式

HRID 2354058 の反応式
[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].OS(O)(=O)=O>>[CH3:8][C:2]1[CH:3]=[C:4]([N+:10]([O-:12])=[O:11])[CH:5]=[C:6]([CH3:7])[N+:1]=1[O-:9]

参加物

4

反応物 3

HCID 944Nitric Acid2 回HCID 1118Sulfuric Acid2 回HCID 140832,6-Dimethylpyridine N-oxide

生成物 1

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

反応条件

温度
80 °C

実験手順

Lutidine-N-oxide (19 g, 155 mmol) is cooled at 0° C. and a mixture of fuming HNO3 (100%, 37.5 mL) and conc. H2SO4 (95-97%, 52.5 mL), prepared by addition of H2SO4 to HNO3 at 0° C., is added slowly. The mixture is heated at 80° C. for 3 h. The cooled mixture is carefully poured into ice-water (500 mL). A white precipitate forms that is filtered. The precipitate is dissolved in CH2Cl2 (100 mL) and the filtrate is extracted with CH2Cl2 (4×75 mL). The organic extracts are combined with the dissolved precipitate and washed with sat. aq. NaCl (2×75 mL), dried (Na2SO4), filtered and evaporated to provide the title compound.

後処理

  1. additionis added slowly
  2. filtrationA white precipitate forms that is filtered
  3. dissolutionThe precipitate is dissolved in CH2Cl2 (100 mL)
  4. extractionthe filtrate is extracted with CH2Cl2 (4×75 mL)
  5. washwashed with sat. aq. NaCl (2×75 mL)
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. customevaporated

出典と根拠

ORDレコード
ord-ab452c8e0e634c79883338a9dd5c08ca
出典データセット
uspto-grants-2010_07
特許番号
US07750161B2

関連ノート

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