2,2’-[(1-甲基亚乙基)二(4,1-亚苯基氧亚甲基)]二环氧乙烷与α-氢-ω-羟基聚(氧-1,2-亚乙基)的聚合物 → 2-(4-溴苯基)-1,3-二氧戊环

HRID 6606

反应方程式

HRID 6606 反应方程式
[Br:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH2:22](O)[CH2:23][OH:24].O>C1C=CC=CC=1.C(OCC)(=O)C>[Br:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]2[O:24][CH2:23][CH2:22][O:7]2)=[CH:4][CH:3]=1

参与物

7

反应物 4

HCID 1742,2’-[(1-甲基亚乙基)二(4,1-亚苯基氧亚甲基)]二环氧乙烷与α-氢-ω-羟基聚(氧-1,2-亚乙基)的聚合物HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 70741对溴苯甲醛HCID 521998对甲苯磺酸水合物

产物 1

HCID 27738422-(4-溴苯基)-1,3-二氧戊环

试剂、催化剂与溶剂 2

HCID 241苯溶剂HCID 8857乙酸乙酯溶剂

实验过程

4-Bromobenzaldehyde (3 g, 0.0162 mol) in benzene (60 mL) was treated with p-toluenesulfonic acid monohydrate (0.15 g, 0.79 mmol) and ethylene glycol (5 mL, 0.0896 mol). The reaction was refluxed under nitrogen with azeotropic removal of water. After 3 hours, the reaction was cooled to room temperature and diluted with an equal volume of ethyl acetate. This solution was washed twice with aqueous bicarbonate, dried over magnesium sulfate and concentrated under reduced pressure. A colorless oil was recovered. Yield=2.83 g (92%). TLC (5% ethyl acetate in hexanes) showed clean product, Rf=0.17.

后处理

  1. washThis solution was washed twice with aqueous bicarbonate
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customA colorless oil was recovered

来源与证据

ORD记录
ord-c0b1f5fc553446359bccb5846409ec6d
来源数据集
uspto-grants-2006_08
专利号
US07083986B2

关联笔记

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