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聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 2-苯甲酰-4-溴苯胺

HRID 463500
笔记
打印预览

反应方程式

HRID 463500 反应方程式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6]([CH:16]=1)=[C:7]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[O:8][N:9]=2.O>[Zn].C(O)(=O)C>[NH2:9][C:5]1[CH:4]=[CH:3][C:2]([Br:1])=[CH:16][C:6]=1[C:7]([C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1)=[O:8]
参与物反应条件实验过程后处理来源与证据反应笔记

参与物

5

反应物 2

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 3472905-溴-3-苯基苯并[C]异噁唑

产物 1

HCID 996772-苯甲酰-4-溴苯胺收率 98.2%

试剂、催化剂与溶剂 2

HCID 23994Zinc催化剂HCID 176醋酸溶剂

反应条件

温度
80 °C

实验过程

5-Bromo-3-phenyl-2,1-benzisoxazole (7.5 g, 28.6 m mol), water (14.6 ml), and zinc dust (9.3 g, 143 m mol) were combined. Acetic acid (8.6 ml, 143 m mol) was added and the mixture was stirred and heated at 80° C. for 90 minutes. After cooling to room temperature, both the liquid and solid portion of the reaction were extracted with methylene chloride. The combined methylene chloride solutions was washed once with sodium hydroxide solution (10%) and several times with water. Drying (sodium sulfate) and evaporation yielded the desired product (7.42 g) of mp. 92°-102° C.

后处理

  1. temperatureAfter cooling to room temperature
  2. extractionthe liquid and solid portion of the reaction were extracted with methylene chloride
  3. washThe combined methylene chloride solutions was washed once with sodium hydroxide solution (10%) and several times with water
  4. customDrying
  5. custom(sodium sulfate) and evaporation

来源与证据

ORD记录
ord-b2acd0f2630d47829bdc8e4459c1340c
来源数据集
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
专利号
US04519938

反应笔记

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本页导航参与物反应条件实验过程后处理来源与证据反应笔记