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聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → Ethyl [(2,2-diethoxyethyl)sulfanyl]acetate

HRID 1061663
笔记
打印预览

反应方程式

HRID 1061663 反应方程式
[O-]CC.[Na+].[C:5]([O:9][CH2:10][CH3:11])(=[O:8])[CH2:6][SH:7].[CH2:12]([O:14][CH:15]([O:18][CH2:19][CH3:20])[CH2:16]Br)[CH3:13].O>C(O)C>[CH2:12]([O:14][CH:15]([O:18][CH2:19][CH3:20])[CH2:16][S:7][CH2:6][C:5]([O:9][CH2:10][CH3:11])=[O:8])[CH3:13]
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 12185巯基乙酸乙酯HCID 74852溴代乙醛缩二乙醇HCID 2723922乙醇钠

产物 1

HCID 22284188Ethyl [(2,2-diethoxyethyl)sulfanyl]acetate收率 58.5%

试剂、催化剂与溶剂 1

HCID 702乙醇溶剂

实验过程

Sodium ethoxide (2.83 g) is added to a solution of ethyl thioglycolate (5.00 g) and bromoacetaldehyde diethylacetal (8.20 g) in ethanol (150 ml), and the mixture is refluxed for three hours. The reaction mixture is allowed to stand at room temperature, water is added to the mixture, and the whole is extracted with diethyl ether. The extract is washed with saturated brine and dried over anhydrous magnesium sulfate. The extract is concentrated under reduced pressure, and the resulting residue is purified by silica gel column chromatography to give the titled reference compound (5.75 g).

后处理

  1. temperaturethe mixture is refluxed for three hours
  2. customto stand at room temperature
  3. extractionthe whole is extracted with diethyl ether
  4. washThe extract is washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationThe extract is concentrated under reduced pressure
  7. customthe resulting residue is purified by silica gel column chromatography

来源与证据

ORD记录
ord-98ee6c5626aa435387c98c317bbb2e7e
来源数据集
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
专利号
US06960575B2

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