1-Methyl-3-aminopyrazole → 1-(1-methyl-1H-pyrazol-3-yl)-2-oxopyrrolidine-3-carbonitrile

HRID 632770

반응식

HRID 632770 반응식
[CH3:1][N:2]1[CH:6]=[CH:5][C:4]([NH2:7])=[N:3]1.[C:8]([C:10]1([C:13](OCC)=[O:14])[CH2:12][CH2:11]1)#[N:9]>COC1CCCC1.C(OCC)(=O)C>[CH3:1][N:2]1[CH:6]=[CH:5][C:4]([N:7]2[CH2:12][CH2:11][CH:10]([C:8]#[N:9])[C:13]2=[O:14])=[N:3]1

참가 물질

5

반응물 2

HCID 1372541-Methyl-3-aminopyrazoleHCID 380810Ethyl 1-cyanocyclopropanecarboxylate

생성물 1

HCID 1180611571-(1-methyl-1H-pyrazol-3-yl)-2-oxopyrrolidine-3-carbonitrile

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 138539Cyclopentyl methyl ether용매

반응 조건

온도
120 °C

실험 절차

To a solution of 1-methyl-1H-pyrazol-3-amine (223 mg) in cyclopentyl methyl ether (5.0 mL) was added ethyl 1-cyanocyclopropanecarboxylate (0.90 ml). The reaction mixture was stirred at 120° C. for 30 hr, and diluted with ethyl acetate. The diluted solution was washed with water and saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (237 mg).

후처리

  1. washThe diluted solution was washed with water and saturated brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. customthe solvent was evaporated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-a0e77610c0bd4d10bae8a39ec29f4fdf
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321757B2

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