Nitric Acid → 4-(Benzyloxy)-5-methoxy-2-nitrobenzonitrile

HRID 896255ノート

反応式

HRID 896255 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[O:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:6]#[N:7].[N+:19]([O-])([OH:21])=[O:20].[K]>C(O)(=O)C>[N+:19]([C:8]1[CH:9]=[C:10]([O:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[C:3]([O:2][CH3:1])=[CH:4][C:5]=1[C:6]#[N:7])([O-:21])=[O:20]

参加物

5

反応物 3

HCID 944Nitric AcidHCID 7937714-Benzyloxy-3-methoxy-benzonitrileHCID 5462222Potassium

生成物 1

HCID 116736184-(Benzyloxy)-5-methoxy-2-nitrobenzonitrile収率 64%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

3-methoxy-4-benzyloxybenzonitrile (4.78 g, 20 mmol) in acetic acid (10 ml) was slowly added to nitric acid (d=1.42, 25 ml) at 20-30° with cooling in an ice bath. The mixture was then stirred at room temperature for 6 hours. The reaction mixture was treated with potassium hydroxyde (10N) at 0° C. The basic mixture (pH 10) was extracted with CH2Cl2, the organic phase was dried over MgSO4, concentrated to give title compound (3.62 g, 64%).

後処理

  1. temperaturewith cooling in an ice bath
  2. extractionThe basic mixture (pH 10) was extracted with CH2Cl2
  3. dry with materialthe organic phase was dried over MgSO4
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-cd1df245d14641e1ba3927a52ac134cd
出典データセット
uspto-grants-2005_07
特許番号
US06919338B2

反応ノート

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