Potassium Nitrate → 4-Methyl-3-nitrobenzotrifluoride

HRID 412079

反応式

HRID 412079 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][CH:3]=1.[N+:12]([O-])([O-:14])=[O:13].[K+].CCCCCC.C(OCC)(=O)C>S(=O)(=O)(O)O>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([F:9])([F:10])[F:11])=[CH:6][C:7]=1[N+:12]([O-:14])=[O:13]

参加物

5

反応物 3

HCID 24434Potassium NitrateHCID 802304-MethylbenzotrifluorideHCID 21226206Ethyl acetate hexane

生成物 1

HCID 14728854-Methyl-3-nitrobenzotrifluoride収率 96%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒2 回

実験手順

To a solution of 4-methylbenzotrifluoride (18.6 g, 116 mmol) in concentrated sulfuric acid (120 ml) was added dropwise a solution of potassium nitrate (12.9 g, 128 mmol) in concentrated sulfuric acid (60 ml) at room temperature over 15 minutes. After stirring for 2 hours at the same temperature, the reaction mixture was poured into ice water, which was extracted with ethyl acetate, dried over anhydrous sodium sulfate, and solvent was distilled off. The residue obtained was submitted to silica gel column chromatography [hexane-ethyl acetate=8:1] to obtain 22.8 g of title compound as pale yellow liquid. Yield 96%.

後処理

  1. extractionwas extracted with ethyl acetate
  2. dry with materialdried over anhydrous sodium sulfate, and solvent
  3. distillationwas distilled off
  4. customThe residue obtained

出典と根拠

ORDレコード
ord-53da0b72a505422f8da21304dfcbc003
出典データセット
uspto-grants-2003_05
特許番号
US06562839B1

関連ノート

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