Water → HCID 86760868, 화합물

HRID 1982971노트

반응식

HRID 1982971 반응식
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]

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 7017727methyl 1-(chloromethyl)-1H-pyrazole-4-carboxylateHCID 10931386HCID 10931386, 화합물

생성물 1

HCID 86760868HCID 86760868, 화합물수율 45.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

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
  7. customrecrystallized from hexane-chloroform

출처 및 근거

ORD 기록
ord-271914447b094c99a1d18c0b685a180f
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07541374B2

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