Water → HCID 86760868、化合物

HRID 1982971ノート

反応式

HRID 1982971 の反応式
Cl[CH2:2][N:3]1[CH:7]=[C:6]([C:8]([O:10][CH3:11])=[O:9])[CH:5]=[N:4]1.[CH2:12]([CH:15]([C:18]#[N:19])[C:16]#[N:17])[CH:13]=[CH2:14].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH2:12]([C:15]([CH2:2][N:3]1[CH:7]=[C:6]([C:8]([O:10][CH3:11])=[O:9])[CH:5]=[N:4]1)([C:18]#[N:19])[C:16]#[N:17])[CH:13]=[CH2:14]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 7017727methyl 1-(chloromethyl)-1H-pyrazole-4-carboxylateHCID 10931386HCID 10931386、化合物

生成物 1

HCID 86760868HCID 86760868、化合物収率 45.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

0.79 g of 1-(chloromethyl)-4-methoxycarbonyl-1H-pyrazole and 0.49 g of allyl malononitrile were dissolved in 15 ml of N,N-dimethylformamide. 1.26 g of potassium carbonate was added to the solution under ice cooling with stirring, followed by stirring at room temperature for overnight. Water was added to the reaction mixture, and then extracted with MTBE. The organic layer was washed with water, dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography, and then recrystallized from hexane-chloroform to obtain 0.50 g of allyl [{4-(methoxycarbonyl)-1H-pyrazole-1-yl}methyl]malononitrile (referred to as the compound of the present invention (24), hereinafter) shown by below formula.

後処理

  1. stirringby stirring at room temperature for overnight
  2. extractionextracted with MTBE
  3. washThe organic layer was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customrecrystallized from hexane-chloroform

出典と根拠

ORDレコード
ord-271914447b094c99a1d18c0b685a180f
出典データセット
uspto-grants-2009_06
特許番号
US07541374B2

反応ノート

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