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

HRID 1982959노트

반응식

HRID 1982959 반응식
Cl[CH2:2][N:3]1[CH:7]=[CH:6][C:5]([C:8]#[N:9])=[N:4]1.[F:10][C:11]([F:20])([F:19])[CH2:12][CH2:13][CH:14]([C:17]#[N:18])[C:15]#[N:16].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[C:8]([C:5]1[CH:6]=[CH:7][N:3]([CH2:2][C:14]([CH2:13][CH2:12][C:11]([F:10])([F:19])[F:20])([C:15]#[N:16])[C:17]#[N:18])[N:4]=1)#[N:9]

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 221857612-(3,3,3-Trifluoropropyl)malononitrileHCID 231491551-(chloromethyl)-3-cyano-1H-pyrazole

생성물 1

HCID 86612645[(3-cyano-1H-pyrazole-1-yl)methyl](3,3,3-trifluoropropyl) malononitrile수율 58.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1.00 g of 1-(chloromethyl)-3-cyano-1H-pyrazole and 1.15 g of (3,3,3-trifluoropropyl) malononitrile were dissolved in 21 ml of N,N-dimethylformamide. 1.96 g of potassium carbonate was added to the solution under ice cooling with stirring, followed by stirring at room temperature for 5 hours. 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 1.11 g of [(3-cyano-1H-pyrazole-1-yl)methyl](3,3,3-trifluoropropyl) malononitrile (referred as the compound of the present invention (9), hereinafter) shown by below formula.

후처리

  1. stirringby stirring at room temperature for 5 hours
  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-6ad4736ed2e946f9a8918ac53005ca4c
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07541374B2

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