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

HRID 230097

反応式

HRID 230097 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-7dad8af06f064827b13d3af25b5e7366
出典データセット
uspto-grants-2009_07
特許番号
US07566683B2

関連ノート

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