Nitric Acid → 3-Ethoxy-2-methyl-6-nitropyridine

HRID 847769

反応式

HRID 847769 の反応式
[CH2:1]([O:3][C:4]1[C:5]([CH3:10])=[N:6][CH:7]=[CH:8][CH:9]=1)[CH3:2].[N+:11]([O-])([OH:13])=[O:12]>S(=O)(=O)(O)O>[CH2:1]([O:3][C:4]1[C:5]([CH3:10])=[N:6][C:7]([N+:11]([O-:13])=[O:12])=[CH:8][CH:9]=1)[CH3:2]

参加物

4

反応物 2

HCID 944Nitric AcidHCID 128750153-Ethoxy-2-methylpyridine2 回

生成物 1

HCID 128750163-Ethoxy-2-methyl-6-nitropyridine

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒2 回

実験手順

To a solution of 70 g of 3-ethoxy-2-methylpyridine (Compound II where R2 =C2H5) dissolved in 280 ml of sulfuric acid under ice-cooling, a mixed solution of 42 ml of fuming nitric acid and 50 ml of concentrated sulfuric acid was added dropwise while stirring and keeping the internal temperature at 0° to 3° C. After stirring for additional 30 minutes at the same temperature, the reaction mixture was poured into ice water and extracted with chloroform. The extract was washed with water, dried over anhydrous sodium sulfate and concentrated to give 85 g of 3-ethoxy-2-methyl-6-nitropyridine (Compound III where R2 =C2H5), m.p. 90°-92° C.

後処理

  1. temperaturecooling
  2. customat 0° to 3° C
  3. stirringAfter stirring for additional 30 minutes at the same temperature
  4. extractionextracted with chloroform
  5. washThe extract was washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-b74d1ccab8e94512af1236e7261d7542
出典データセット
uspto-grants-1981_10
特許番号
US04293695

関連ノート

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