聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → HCID 14012477，化合物

HRID 568614笔记

反应方程式

HRID 568614 反应方程式
Cl[C:2]1[C:16]([Cl:17])=[C:15]([OH:18])[CH:14]=[CH:13][C:3]=1[C:4](=[N:11][OH:12])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[H-].[Na+].Br[CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24].O>CN(C)C=O.C1(C)C=CC=CC=1>[CH2:26]([O:25][C:23](=[O:24])[CH2:22][O:18][C:15]1[CH:14]=[CH:13][C:3]2[C:4]([C:5]3[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=3)=[N:11][O:12][C:2]=2[C:16]=1[Cl:17])[CH3:27]

参与物

7

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 7748溴乙酸乙酯HCID 24758氢化钠2 次HCID 136393678HCID 136393678，化合物

产物 1

HCID 14012477HCID 14012477，化合物

试剂、催化剂与溶剂 2

HCID 1140甲苯溶剂HCID 6228N,N-二甲基甲酰胺溶剂2 次

实验过程

A solution of 2,3-dichloro-4-hydroxybenzophenone oxime and 2.6 g of sodium hydride in 50 ml of dimethylformamide and 50 ml of toluene is heated to 118° C. and maintained at this temperature for 50 minutes. Thereafter, the reaction is permitted to cool prior to the dropwise addition of 7.9 g of ethyl bromoacetate in 50 ml of dimethylformamide. After the addition is complete the reaction mixture is stirred at ambient temperature for 40 minutes. To the well stirred mixture water is added dropwise to decompose any excess sodium hydride. The toluene is evaporated under vacuum and the resulting precipitate is collected by filtration and then rinsed with ether to yield the product ethyl[(7-chloro-3-phenyl-1,2-benzisoxazol-6-yl)oxy]acetate having a melting point of 130° to 132° C.

后处理

  1. temperaturemaintained at this temperature for 50 minutes
  2. temperatureto cool
  3. additionAfter the addition
  4. additionis added dropwise
  5. customThe toluene is evaporated under vacuum
  6. filtrationthe resulting precipitate is collected by filtration
  7. washrinsed with ether

来源与证据

ORD记录
ord-6fd268a9c34d45ee8782c940b997e608
来源数据集
uspto-grants-1988_03
专利号
US04728662

反应笔记

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