m-Chloroperbenzoic acid → 2-(2-Methoxy-4-trifluoromethoxy-phenyl)-3-methyl-5-nitro-pyridine 1-oxide

HRID 2179997노트

반응식

HRID 2179997 반응식
C1C=C(Cl)C=C(C(OO)=[O:9])C=1.[CH3:12][O:13][C:14]1[CH:19]=[C:18]([O:20][C:21]([F:24])([F:23])[F:22])[CH:17]=[CH:16][C:15]=1[C:25]1[C:30]([CH3:31])=[CH:29][C:28]([N+:32]([O-:34])=[O:33])=[CH:27][N:26]=1>C(Cl)Cl>[CH3:12][O:13][C:14]1[CH:19]=[C:18]([O:20][C:21]([F:24])([F:22])[F:23])[CH:17]=[CH:16][C:15]=1[C:25]1[C:30]([CH3:31])=[CH:29][C:28]([N+:32]([O-:34])=[O:33])=[CH:27][N+:26]=1[O-:9]

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 224900532-(2-Methoxy-4-trifluoromethoxy-phenyl)-3-methyl-5-nitro-pyridine

생성물 1

HCID 224900552-(2-Methoxy-4-trifluoromethoxy-phenyl)-3-methyl-5-nitro-pyridine 1-oxide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

MCPBA (78.26 g, 0.349 mol) is added to a solution of 2-(2-methoxy-4-trifluoromethoxy-phenyl)-3-methyl-5-nitro-pyridine (95.6 g, 0.291 mol) in CH2Cl2 (500 ml) at room temperature. The mixture is stirred at room temperature for 3 hours. (1.2 L) and hexane (300 ml) and the mixture is washed with saturated aqueous Na2CO3 and brine. After drying over Na2SO4, the solvent is removed under reduced pressure to give 2-(2methoxy-4-trifluoromethoxy-phenyl)-3-methyl-5-nitro-pyridine 1-oxide as yellow solid. Rf (hexane/EtOAc=1:1)=0.40.

후처리

  1. wash(1.2 L) and hexane (300 ml) and the mixture is washed with saturated aqueous Na2CO3 and brine
  2. dry with materialAfter drying over Na2SO4
  3. customthe solvent is removed under reduced pressure

출처 및 근거

ORD 기록
ord-2533471316b74b5dbddfa835556694f0
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06887875B2

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