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

HRID 230082
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HRID 230082 반응식
[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]
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참가 물질

5

반응물 3

HCID 7856ChloroacetonitrileHCID 11430Potassium CarbonateHCID 178505719HCID 178505719, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3ed4533132e7444dbe7feed887ba50f9
출처 데이터셋
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07566683B2

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