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

HRID 632770

反応式

HRID 632770 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 138539Cyclopentyl methyl ether溶媒

反応条件

温度
120 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-a0e77610c0bd4d10bae8a39ec29f4fdf
出典データセット
uspto-grants-2016_04
特許番号
US09321757B2

関連ノート

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