Potassium Nitrate → 4-Methyl-3-nitrobenzotrifluoride

HRID 412079

반응식

HRID 412079 반응식
[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]

참가 물질

5

반응물 3

HCID 24434Potassium NitrateHCID 802304-MethylbenzotrifluorideHCID 21226206Ethyl acetate hexane

생성물 1

HCID 14728854-Methyl-3-nitrobenzotrifluoride수율 96%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

실험 절차

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%.

후처리

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

출처 및 근거

ORD 기록
ord-53da0b72a505422f8da21304dfcbc003
출처 데이터셋
uspto-grants-2003_05
특허 번호
US06562839B1

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