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

HRID 230097

반응식

HRID 230097 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-7dad8af06f064827b13d3af25b5e7366
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07566683B2

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