Water → [5-(2-fluoro-1-fluoromethyl-1-methyl-ethyl)-2-p-tolyl-2H-pyrazol-3-yl]-carbamic acid 2,2,2-trichloro-ethyl ester

HRID 729603노트

반응식

HRID 729603 반응식
Cl[C:2]([O:4][CH2:5][C:6]([Cl:9])([Cl:8])[Cl:7])=[O:3].C(=O)([O-])[O-].[Na+].[Na+].[F:16][CH2:17][C:18]([C:22]1[CH:23]=[C:24]([NH2:34])[N:25]([C:27]2[CH:32]=[CH:31][C:30]([CH3:33])=[CH:29][CH:28]=2)[N:26]=1)([CH2:20][F:21])[CH3:19].O>C1COCC1>[Cl:7][C:6]([Cl:9])([Cl:8])[CH2:5][O:4][C:2](=[O:3])[NH:34][C:24]1[N:25]([C:27]2[CH:28]=[CH:29][C:30]([CH3:33])=[CH:31][CH:32]=2)[N:26]=[C:22]([C:18]([CH2:17][F:16])([CH3:19])[CH2:20][F:21])[CH:23]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 870632,2,2-Trichloroethyl chloroformateHCID 685380205-(2-fluoro-1-fluoromethyl-1-methyl-ethyl)-2-p-tolyl-2H-pyrazol-3-ylamine

생성물 1

HCID 68538054[5-(2-fluoro-1-fluoromethyl-1-methyl-ethyl)-2-p-tolyl-2H-pyrazol-3-yl]-carbamic acid 2,2,2-trichloro-ethyl ester

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Add 2,2,2-trichloroethyl chloroformate (8.1 mmol, 1.1 mL) and aqueous sodium carbonate solution (4.8 mL) over a solution of 5-(2-fluoro-1-fluoromethyl-1-methyl-ethyl)-2-p-tolyl-2H-pyrazol-3-ylamine (7.3 mmol, 1.9 g) in 37 mL of THF. Stir for 24 hours. Pour the solution over water and extract in ethyl acetate. Combine organic layers and wash with saturated aq. sodium chloride. Dry over sodium sulfate, filter, and concentrate under reduced pressure to give [5-(2-fluoro-1-fluoromethyl-1-methyl-ethyl)-2-p-tolyl-2H-pyrazol-3-yl]-carbamic acid 2,2,2-trichloro-ethyl ester. LCMS ES+ (m/z) 440 [M+H].

후처리

  1. extractionextract in ethyl acetate
  2. washCombine organic layers and wash with saturated aq. sodium chloride
  3. dry with materialDry over sodium sulfate
  4. filtrationfilter
  5. concentrationconcentrate under reduced pressure

출처 및 근거

ORD 기록
ord-2d68bfde4de44eaea10fea61ef90d66d
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07582638B2

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