Hydrogen Peroxide → 2-(Trifluoromethyl)pyridine 1-oxide

HRID 1810988노트

반응식

HRID 1810988 반응식
[F:1][C:2]([F:10])([F:9])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1.[OH:11]O>C(O)(=O)C>[F:1][C:2]([F:10])([F:9])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N+:4]=1[O-:11]

참가 물질

4

반응 조건

온도
70 °C

실험 절차

To a stirred solution of 2-trifluoromethyl pyridine (5 g, 34 mmol) in acetic acid (25 mL) is added 33% of aqueous H2O2 (20 mL) at room temperature. The reaction mixture is allowed to stir for 12 h at 70° C. After complete consumption of starting material the reaction mixture is concentrated under reduced pressure. The residue is dissolved in chloroform (250 mL) and pH is adjusted to 7 with K2CO3 (20 g approx). Resulting solid is filtered through glass sintered funnel and washed with chloroform. Filtrate is concentrated under reduced pressure to give 2-trifluoromethyl-pyridine 1-oxide as syrupy liquid (4.3 g).

후처리

  1. customAfter complete consumption of starting material the reaction mixture
  2. concentrationis concentrated under reduced pressure
  3. dissolutionThe residue is dissolved in chloroform (250 mL)
  4. customResulting solid
  5. filtrationis filtered through glass sintered funnel
  6. washwashed with chloroform
  7. concentrationFiltrate is concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-595de53777d74446aa43ab85662dfa98
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08362249B2

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