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聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → HCID 86612665,化合物

HRID 1982979
笔记
打印预览

反应方程式

HRID 1982979 反应方程式
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]
参与物实验过程后处理来源与证据反应笔记

参与物

6

反应物 4

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 11430碳酸钾HCID 221857612-(3,3,3-Trifluoropropyl)malononitrileHCID 23149134HCID 23149134,化合物

产物 1

HCID 86612665HCID 86612665,化合物收率 9.4%

试剂、催化剂与溶剂 1

HCID 6228N,N-二甲基甲酰胺溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-e737165b341f418f842c400d6d63981c
来源数据集
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
专利号
US07541374B2

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记