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

HRID 1982960노트

반응식

HRID 1982960 반응식
Cl.Cl[CH2:3][N:4]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[N:5]1.[F:15][C:16]([F:25])([F:24])[CH2:17][CH2:18][CH:19]([C:22]#[N:23])[C:20]#[N:21].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[C:9]1([C:6]2[CH:7]=[CH:8][N:4]([CH2:3][C:19]([CH2:18][CH2:17][C:16]([F:15])([F:24])[F:25])([C:20]#[N:21])[C:22]#[N:23])[N:5]=2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 221857612-(3,3,3-Trifluoropropyl)malononitrileHCID 231491981-(chloromethyl)-3-phenyl-1H-pyrazole hydrochloride

생성물 1

HCID 86612646[(3-phenyl-1H-pyrazole-1-yl)methyl](3,3,3-trifluoropropyl)malononitrile수율 23.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2.01 g of 1-(chloromethyl)-3-phenyl-1H-pyrazole hydrochloride and 1.42 g of (3,3,3-trifluoropropyl) malononitrile were dissolved in 27 ml of N,N-dimethylformamide. 2.43 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 to obtain 0.66 g of [(3-phenyl-1H-pyrazole-1-yl)methyl](3,3,3-trifluoropropyl)malononitrile (referred as the compound of the present invention (10), hereinafter) shown by below formula.

후처리

  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

출처 및 근거

ORD 기록
ord-4785ff41c3054008b131bedaa9e95709
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07541374B2

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