Water → [(3-i-propyl-1H-pyrazole-1-yl)methyl](3,3,3-trifluoropropyl) malononitrile

HRID 1982952ノート

反応式

HRID 1982952 の反応式
Cl.[CH:2]([C:5]1[CH:9]=[CH:8][N:7]([CH2:10]Cl)[N:6]=1)([CH3:4])[CH3:3].[F:12][C:13]([F:22])([F:21])[CH2:14][CH2:15][CH:16]([C:19]#[N:20])[C:17]#[N:18].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH:2]([C:5]1[CH:9]=[CH:8][N:7]([CH2:10][C:16]([CH2:15][CH2:14][C:13]([F:12])([F:21])[F:22])([C:17]#[N:18])[C:19]#[N:20])[N:6]=1)([CH3:4])[CH3:3]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 221857612-(3,3,3-Trifluoropropyl)malononitrileHCID 231491783-i-propyl-1-(chloromethyl)-1H-pyrazole hydrochloride

生成物 1

HCID 11277575[(3-i-propyl-1H-pyrazole-1-yl)methyl](3,3,3-trifluoropropyl) malononitrile収率 37.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

0.77 g of 3-i-propyl-1-(chloromethyl)-1H-pyrazole hydrochloride and 0.64 g of (3,3,3-trifluoropropyl)malononitrile were dissolved in 8 ml of N,N-dimethylformamide. 1.54 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-ethyl acetate to obtain 0.42 g of [(3-i-propyl-1H-pyrazole-1-yl)methyl](3,3,3-trifluoropropyl) malononitrile (referred as the compound of the present invention (2), 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-ethyl acetate

出典と根拠

ORDレコード
ord-a8465bcb5d384c8eaee56259137373ab
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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