Nitric Acid → HCID 22019211、化合物

HRID 6890ノート

反応式

HRID 6890 の反応式
[N+:1]([O-:4])(O)=[O:2].[CH3:5][C:6]1[CH:7]=[N:8][CH:9]=[CH:10][C:11]=1[O:12][CH3:13].C(=O)([O-])[O-].[K+].[K+]>S(=O)(=O)(O)O>[CH3:5][C:6]1[CH:7]=[N:8][CH:9]=[C:10]([N+:1]([O-:4])=[O:2])[C:11]=1[O:12][CH3:13]

参加物

5

反応物 3

HCID 944Nitric AcidHCID 11430Potassium Carbonate2 回HCID 47377664-Methoxy-3-methylpyridine

生成物 1

HCID 22019211HCID 22019211、化合物収率 30%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

30 ml of 100% nitric acid is added to 150 ml of 98% sulphuric acid with stirring and cooling. To this solution is added dropwise 3.2 g (26 mmol) of 3-methyl-4-methoxy pyridine. The mixture is stirred at 80° C. for 2.5 hours, cooled down and added cautiously to a mixture of 400 g of crushed ice and 300 g of potassium carbonate with external cooling. 125 g more of potassium carbonate is added, and the suspension is filtered. The cake is washed with around 1 l of diethyl ether. The filtrate layers are separated, the ethereal layer is dried, filtered off and concentrated to give 2.9 g (30% yield) of a yellow oil (M+1 =169) (purity #80%, used with no further purification).

後処理

  1. temperaturecooling
  2. stirringThe mixture is stirred at 80° C. for 2.5 hours
  3. temperaturecooled down
  4. filtrationthe suspension is filtered
  5. washThe cake is washed with around 1 l of diethyl ether
  6. customThe filtrate layers are separated
  7. customthe ethereal layer is dried
  8. filtrationfiltered off
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-082f5c4b45dc497e883bc6aabeb2e2b5
出典データセット
uspto-grants-2006_08
特許番号
US07084163B2

反応ノート

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