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Chloroacetonitrile → 1-Cyanomethyl-3-(2,6-difluorophenyl)pyrazole

HRID 230082
ノート
印刷プレビュー

反応式

HRID 230082 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[C:9]1[CH:13]=[CH:12][NH:11][N:10]=1.Cl[CH2:15][C:16]#[N:17].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[C:16]([CH2:15][N:11]1[CH:12]=[CH:13][C:9]([C:3]2[C:4]([F:8])=[CH:5][CH:6]=[CH:7][C:2]=2[F:1])=[N:10]1)#[N:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7856ChloroacetonitrileHCID 11430Potassium CarbonateHCID 178505719HCID 178505719、化合物

生成物 1

HCID 221694981-Cyanomethyl-3-(2,6-difluorophenyl)pyrazole収率 47.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

3.0 g of 3-(2,6-difluorophenyl)pyrazole was dissolved in 20 ml of acetonitrile, and 2.52 g of chloroacetonitrile and 4.61 g of potassium carbonate were added thereto at room temperature, and heated under reflux for 5 hours. After acetonitrile was distilled off under reduced pressure, ethyl acetate was added to the residue, which was then washed with a small amount of water. The organic layer was dried over sodium sulfate, and the solvent was distilled off under reduced pressure. The residual product was recrystallized from a mixed solvent of isopropylether and diethyl ether to obtain 1.74 g of 1-cyanomethyl-3-(2,6-difluorophenyl)pyrazole.

後処理

  1. temperatureunder reflux for 5 hours
  2. distillationAfter acetonitrile was distilled off under reduced pressure, ethyl acetate
  3. additionwas added to the residue, which
  4. washwas then washed with a small amount of water
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residual product was recrystallized from a mixed solvent of isopropylether and diethyl ether

出典と根拠

ORDレコード
ord-3ed4533132e7444dbe7feed887ba50f9
出典データセット
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07566683B2

反応ノート

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