Water → allyl [(4-chloro-1H-pyrazole-1-yl)methyl]malononitrile

HRID 1982967노트

반응식

HRID 1982967 반응식
Cl.[Cl:2][C:3]1[CH:4]=[N:5][N:6]([CH2:8]Cl)[CH:7]=1.[CH2:10]([CH:13]([C:16]#[N:17])[C:14]#[N:15])[CH:11]=[CH2:12].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH2:10]([C:13]([CH2:8][N:6]1[CH:7]=[C:3]([Cl:2])[CH:4]=[N:5]1)([C:16]#[N:17])[C:14]#[N:15])[CH:11]=[CH2:12]

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 10931386HCID 10931386, 화합물HCID 231491194-chloro-1-(chloromethyl)-1H-pyrazole hydrochloride

생성물 1

HCID 86612655allyl [(4-chloro-1H-pyrazole-1-yl)methyl]malononitrile수율 72.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1.43 g of 4-chloro-1-(chloromethyl)-1H-pyrazole hydrochloride and 1.01 g of allyl malononitrile were dissolved in 30 ml of N,N-dimethylformamide. 2.76 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 1.22 g of allyl [(4-chloro-1H-pyrazole-1-yl)methyl]malononitrile (referred as the compound of the present invention (20), 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-ec93892cb8444a498fe11f3e35ff6f82
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07541374B2

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