聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 2-Amino-3-(4-chlorocinnamylamino)pyridine

HRID 5735

反应方程式

HRID 5735 反应方程式
[Cl:1][C:2]1[CH:11]=[CH:10][C:5]([CH:6]=[CH:7][CH2:8]Cl)=[CH:4][CH:3]=1.[NH2:12][C:13]1[C:18]([NH2:19])=[CH:17][CH:16]=[CH:15][N:14]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[NH2:12][C:13]1[C:18]([NH:19][CH2:8][CH:7]=[CH:6][C:5]2[CH:10]=[CH:11][C:2]([Cl:1])=[CH:3][CH:4]=2)=[CH:17][CH:16]=[CH:15][N:14]=1

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 99562,3-二氨基吡啶HCID 11430碳酸钾HCID 53728250p-Chlorocinnamyl chloride

产物 1

HCID 542524182-Amino-3-(4-chlorocinnamylamino)pyridine收率 42.2%

试剂、催化剂与溶剂 1

HCID 6228N,N-二甲基甲酰胺溶剂

实验过程

7.71 g of p-chlorocinnamyl chloride and 13.5 g of 2,3-diaminopyridine were dissolved in 220 ml of dimethylformamide, and to the solution was added 8.6 g of potassium carbonate, and the mixture was stirred at a room temperature for 50 hours, and after adding 300 ml of water, extracted twice with 200 ml of chloroform. The extract was dried over magnesium sulfate and concentrated under a reduced pressure, and resulting residue was applied to a silica gel column and eluted with chloroform/methanol (100:1 to 50:1), to obtain 4.52 g of the title compound as yellow crystals.

后处理

  1. extractionextracted twice with 200 ml of chloroform
  2. dry with materialThe extract was dried over magnesium sulfate
  3. concentrationconcentrated under a reduced pressure
  4. customresulting residue
  5. washeluted with chloroform/methanol (100:1 to 50:1)

来源与证据

ORD记录
ord-d4ee0e39c1e94258bf77463d69e44f83
来源数据集
uspto-grants-1993_09
专利号
US05245034

关联笔记

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