Nitric Acid → HCID 22019211、化合物

HRID 1442894ノート

反応式

HRID 1442894 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 11 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 11 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-0d80e3031c37456699b12033f46d0ee1
出典データセット
uspto-grants-2010_02
特許番号
US07659307B2

反応ノート

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