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

HRID 1357436ノート

反応式

HRID 1357436 の反応式
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

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 527610Prop-2-enyl 2-bromoacetateHCID 178505719HCID 178505719、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-a7bc402cded647e5b56174a0c21f7090
出典データセット
uspto-grants-2003_07
特許番号
USRE038188E1

反応ノート

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