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聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → [(3-t-butyl-1H-pyrazole-1-yl)methyl](3,3,3-trifluoropropyl) malononitrile

HRID 1982953
笔记
打印预览

反应方程式

HRID 1982953 反应方程式
Cl.[C:2]([C:6]1[CH:10]=[CH:9][N:8]([CH2:11]Cl)[N:7]=1)([CH3:5])([CH3:4])[CH3:3].[F:13][C:14]([F:23])([F:22])[CH2:15][CH2:16][CH:17]([C:20]#[N:21])[C:18]#[N:19].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[C:2]([C:6]1[CH:10]=[CH:9][N:8]([CH2:11][C:17]([CH2:16][CH2:15][C:14]([F:13])([F:22])[F:23])([C:18]#[N:19])[C:20]#[N:21])[N:7]=1)([CH3:5])([CH3:4])[CH3:3]
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 231491523-t-butyl-1-(chloromethyl)-1H-pyrazole hydrochloride

产物 1

HCID 86612639[(3-t-butyl-1H-pyrazole-1-yl)methyl](3,3,3-trifluoropropyl) malononitrile收率 38.1%

试剂、催化剂与溶剂 1

HCID 6228
N,N-二甲基甲酰胺
溶剂

实验过程

1.16 g of 3-t-butyl-1-(chloromethyl)-1H-pyrazole hydrochloride and 0.98 g of (3,3,3-trifluoropropyl)malononitrile were dissolved in 17 ml of N,N-dimethylformamide. 1.54 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 0.63 g of [(3-t-butyl-1H-pyrazole-1-yl)methyl](3,3,3-trifluoropropyl) malononitrile (referred as the compound of the present invention (3), 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-62527dd35d8d4cdebb41dcaaebca0c50
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