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Water → HCID 86612665, 화합물

HRID 1982979
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HRID 1982979 반응식
Cl[CH2:2][N:3]1[CH:7]=[N:6][C:5]([C:8]([F:14])([F:13])[C:9]([F:12])([F:11])[F:10])=[N:4]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>[F:13][C:8]([F:14])([C:5]1[N:6]=[CH:7][N:3]([CH2:2][C:19]([CH2:18][CH2:17][C:16]([F:15])([F:24])[F:25])([C:20]#[N:21])[C:22]#[N:23])[N:4]=1)[C:9]([F:12])([F:11])[F:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 221857612-(3,3,3-Trifluoropropyl)malononitrileHCID 23149134HCID 23149134, 화합물

생성물 1

HCID 86612665HCID 86612665, 화합물수율 9.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1.74 g of 1-(chloromethyl)-3-(pentafluoroethyl)-1H-1,2,4-triazole and 1.20 g of (3,3,3-trifluoropropyl)malononitrile were dissolved in 21 ml of N,N-dimethylformamide. 2.04 g of potassium carbonate was added to the solution under ice cooling with stirring, followed by stirring at room temperature for 4 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 recrystallized from hexane-MTBE to obtain 0.25 g of {[3-(pentafluoroethyl)-1H-1,2,4-triazole 1-yl]methyl}(3,3,3-trifluoropropyl) malononitrile (referred as the compound of the present invention (34), hereinafter) shown by below formula.

후처리

  1. stirringby stirring at room temperature for 4 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
  7. customThe residue was recrystallized from hexane-MTBE

출처 및 근거

ORD 기록
ord-e737165b341f418f842c400d6d63981c
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07541374B2

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