四溴化碳 → 5-(2,2-Dibromoethenyl)-2,2'-bithiophene

HRID 1289114

反应方程式

HRID 1289114 反应方程式
[CH:1]([C:3]1[S:7][C:6]([C:8]2[S:9][CH:10]=[CH:11][CH:12]=2)=[CH:5][CH:4]=1)=O.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.[C:32](Br)(Br)([Br:34])[Br:33].C(C1SC(C2SC=CC=2)=CC=1)=O.ClCCl>ClCCl.CCCCCC>[Br:33][C:32]([Br:34])=[CH:1][C:3]1[S:7][C:6]([C:8]2[S:9][CH:10]=[CH:11][CH:12]=2)=[CH:5][CH:4]=1

参与物

7

反应物 4

HCID 11205四溴化碳HCID 11776三苯基膦HCID 3644282，2-联噻吩-5-乙醛HCID 867503605-Formyl-2,2'-bithiophene dichloromethane

产物 1

HCID 131139775-(2,2-Dibromoethenyl)-2,2'-bithiophene

试剂、催化剂与溶剂 2

HCID 6344二氯甲烷溶剂2 次HCID 8058正己烷溶剂

实验过程

0.55 g of 5-formyl-2,2'-bithiophene was dissolved in 10 ml of dichloromethane. 1.95 g of PPh3 and 1.23 g of CBr4 were dissolved in 40 ml of dichloromethane and mixed with the 5-formyl-2,2'-bithiophene/dichloromethane solution under nitrogen gas atmosphere at 0° C. After the mixture was stirred for 1 hour and 10 ml of n-hexane was added to precipitate the triphenyl-phosphine oxide. And the reaction solution was filtered. Further, 100 ml of n-hexane was then added into the solution and the yellowish solid was obtained. The solid was further purified by column chromatography and crystallized with ethanol. The crystal product was thus obtained and the melting point thereof was 112°-113° C.

后处理

  1. customto precipitate the triphenyl-phosphine oxide
  2. filtrationAnd the reaction solution was filtered
  3. additionFurther, 100 ml of n-hexane was then added into the solution
  4. customthe yellowish solid was obtained
  5. customThe solid was further purified by column chromatography
  6. customcrystallized with ethanol
  7. customThe crystal product was thus obtained
  8. customthereof was 112°-113° C.

来源与证据

ORD记录
ord-a5690e8d0f9b4ac99af0fe15e7a246fa
来源数据集
uspto-grants-1998_05
专利号
US05747525

关联笔记

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