Diethyl (ethoxymethylene)malonate → Diethyl 2-([[3-methyl-1-(2-pyridinyl)-1H-pyrazol-5-yl]amino]methylene)malonate

HRID 497934

反応式

HRID 497934 の反応式
C(O[CH:4]=[C:5]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[C:6]([O:8][CH2:9][CH3:10])=[O:7])C.[CH3:16][C:17]1[CH:21]=[C:20]([NH2:22])[N:19]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=2)[N:18]=1>>[CH3:16][C:17]1[CH:21]=[C:20]([NH:22][CH:4]=[C:5]([C:6]([O:8][CH2:9][CH3:10])=[O:7])[C:11]([O:13][CH2:14][CH3:15])=[O:12])[N:19]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=2)[N:18]=1

参加物

3

反応物 2

HCID 6871Diethyl (ethoxymethylene)malonateHCID 7351323-Methyl-1-(pyridin-2-yl)-1H-pyrazol-5-amine

生成物 1

HCID 22320362Diethyl 2-([[3-methyl-1-(2-pyridinyl)-1H-pyrazol-5-yl]amino]methylene)malonate収率 96%

反応条件

温度
120 °C

実験手順

A mixture of diethyl ethoxymethylenemalonate (32.5 g, 0.15 mol) and 3-methyl-1-(2-pyridinyl)-1H-pyrazol-5-amine (23.8 g, 0.137 mol) was heated under reflux at 120° C. for 1 hour. After the mixture was allowed to cool to room temperature, the reaction solvent was evaporated under reduced pressure. The crude crystals thus obtained were filtered and washed with diethylether to give the title compound (45 g, 96% yield).

後処理

  1. temperaturewas heated
  2. temperatureto cool to room temperature
  3. customthe reaction solvent was evaporated under reduced pressure
  4. customThe crude crystals thus obtained
  5. filtrationwere filtered
  6. washwashed with diethylether

出典と根拠

ORDレコード
ord-34b8fc18d8c74f8bba3d7ab89fdd719a
出典データセット
uspto-grants-2005_09
特許番号
US06949648B2

関連ノート

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