Acetic Acid → 4-Methyl-2-nitrobenzoic acid

HRID 2358648

反応式

HRID 2358648 の反応式
[CH3:1][C:2]1[CH:9]=[CH:8]C(C#N)=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=1.OS(O)(=O)=O.[CH3:18][C:19]([OH:21])=[O:20]>>[CH3:1][C:2]1[CH:9]=[CH:8][C:18]([C:19]([OH:21])=[O:20])=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=1

参加物

4

反応物 3

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 962352-Nitro-4-toluonitrile

生成物 1

HCID 2550274-Methyl-2-nitrobenzoic acid収率 87%

実験手順

A suspension of 4-methyl-2-nitrobenzonitrile (5.00 g, 30.8 mmol) and 50% H2SO4 (25 mL) in HOAc (25 mL) was heated to reflux for 22 h. The reaction mixture was poured into ice-water (150 g) under stirring and stirred at 5° C. for 30 minutes. The deposited crystals were collected by filtration, washed with H2O and n-hexane, and dried at 40° C. in vacuum to give the title compound as pale brown crystal (4.85 g, 87%).

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 22 h
  3. stirringstirred at 5° C. for 30 minutes
  4. filtrationThe deposited crystals were collected by filtration
  5. washwashed with H2O and n-hexane
  6. customdried at 40° C. in vacuum

出典と根拠

ORDレコード
ord-bef22fc7a29a429398661fa4f18eb708
出典データセット
uspto-grants-2010_07
特許番号
US07763731B2

関連ノート

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