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聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → HCID 86612666,化合物

HRID 1982980
笔记
打印预览

反应方程式

HRID 1982980 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.[CH2:15]([CH:18]([C:21]#[N:22])[C:19]#[N:20])[CH:16]=[CH2:17].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH2:15]([C:18]([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)([C:21]#[N:22])[C:19]#[N:20])[CH:16]=[CH2:17]
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 10931386HCID 10931386,化合物HCID 23149134HCID 23149134,化合物

产物 1

HCID 86612666HCID 86612666,化合物

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-(chloromethyl)-3-(pentafluoroethyl)-1H-1,2,4-triazole and 1.02 g of allyl malononitrile were dissolved in 28 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, and then subjected to preparative high performance liquid chromatography to obtain 0.54 g of allyl {[3-(pentafluoroethyl)-1H-1,2,4-triazole 1-yl]methyl}malononitrile (referred as the compound of the present invention (35), hereinafter) shown by below formula.

后处理

  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

来源与证据

ORD记录
ord-e641bc190ef24d2a93f61bb2617f2eb8
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