Potassium Carbonate → Allyl 2-(3-(2,6-difluorophenyl)pyrazol-1-yl)acetate

HRID 1357436노트

반응식

HRID 1357436 반응식
C(=O)([O-])[O-].[K+].[K+].[F:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([F:14])[C:9]=1[C:15]1[CH:19]=[CH:18][NH:17][N:16]=1.Br[CH2:21][C:22]([O:24][CH2:25][CH:26]=[CH2:27])=[O:23]>C(#N)C>[F:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([F:14])[C:9]=1[C:15]1[CH:19]=[CH:18][N:17]([CH2:21][C:22]([O:24][CH2:25][CH:26]=[CH2:27])=[O:23])[N:16]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 527610Prop-2-enyl 2-bromoacetateHCID 178505719HCID 178505719, 화합물

생성물 1

HCID 22169508Allyl 2-(3-(2,6-difluorophenyl)pyrazol-1-yl)acetate수율 97.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Potassium carbonate (1.53 g) was added to an acetonitrile (10 mL) solution of 3-(2,6-difluorophenyl)-pyrazole (1 g) and allyl 2-bromoacetate (1.49 g), and refluxed for 3 hours. The resulting product was extracted with acetate and diluted hydrochloric acid added thereto at room temperature. The organic layer was dried over anhydrous magnesium sulfate and concentrated, and the resulting concentrate was purified through silica gel column chromatography (chloroform) to obtain allyl 2-{3-(2,6-difluorophenyl) pyrazol-1-yl}acetate (1.5 g).

후처리

  1. temperaturerefluxed for 3 hours
  2. extractionThe resulting product was extracted with acetate and diluted hydrochloric acid
  3. additionadded
  4. customat room temperature
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. concentrationthe resulting concentrate
  8. customwas purified through silica gel column chromatography (chloroform)

출처 및 근거

ORD 기록
ord-a7bc402cded647e5b56174a0c21f7090
출처 데이터셋
uspto-grants-2003_07
특허 번호
USRE038188E1

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