Water → Methyl {o-{5-{[1-methyl-5-(trifluoromethyl)pyrazol-3-yl]oxy}-2-nitrophenoxy}phenoxy}acetate

HRID 21518노트

반응식

HRID 21518 반응식
F[C:2]1[CH:3]=[CH:4][C:5]([N+:21]([O-:23])=[O:22])=[C:6]([CH:20]=1)[O:7][C:8]1[CH:19]=[CH:18][CH:17]=[CH:16][C:9]=1[O:10][CH2:11][C:12]([O:14][CH3:15])=[O:13].[CH3:24][N:25]1[C:29]([C:30]([F:33])([F:32])[F:31])=[CH:28][C:27]([OH:34])=[N:26]1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O.C(OCC)(=O)C>[CH3:24][N:25]1[C:29]([C:30]([F:31])([F:32])[F:33])=[CH:28][C:27]([O:34][C:2]2[CH:3]=[CH:4][C:5]([N+:21]([O-:23])=[O:22])=[C:6]([CH:20]=2)[O:7][C:8]2[CH:19]=[CH:18][CH:17]=[CH:16][C:9]=2[O:10][CH2:11][C:12]([O:14][CH3:15])=[O:13])=[N:26]1

참가 물질

7

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 54233795Methyl [o-(5-fluoro-2-nitrophenoxy)phenoxy]acetateHCID 178481944HCID 178481944, 화합물

생성물 1

HCID 57199828Methyl {o-{5-{[1-methyl-5-(trifluoromethyl)pyrazol-3-yl]oxy}-2-nitrophenoxy}phenoxy}acetate수율 31.5%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
100 °C

실험 절차

A mixture of methyl [o-(5-fluoro-2-nitrophenoxy)phenoxy]acetate (1.1 g, 3.4 mmol), 1-methyl-5-(trifluoromethyl)pyrazol-3-ol (0.63 g, 3.8 mmol) and potassium carbonate (0.53 g, 3.8 mmol) in N,N-dimethylformamide is stirred at 100° C. for 18 hours, cooled to room temperature, poured into water and extracted with ethyl acetate. The organic extract is washed with brine, dried over anhydrous sodium sulfate and concentrated in vacuo to obtain an orange oil. Column chromatography of the oil using silica gel and a 30% ethyl acetate in hexanes solution gives the title product as a yellow oil (0.5 g) which is identified by 1HNMR and 13CNMR spectral analyses.

후처리

  1. temperaturecooled to room temperature
  2. extractionextracted with ethyl acetate
  3. extractionThe organic extract
  4. washis washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customto obtain an orange oil

출처 및 근거

ORD 기록
ord-46647fc881914ca98a879d80d107cc7d
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05424280

반응 노트

불러오는 중…