HRID217423

反应详情

EQUATION

反应方程式

HRID 217423 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a solution of methyl 5-bromo-4-phenylthiophene-2-carboxylate in dioxane were added 2-isopropenyl-4,4,5,5-tetramethyl 1,3,2-dioxaborolane and a 2 M aqueous Na2CO3 solution. To the reaction mixture were added palladium acetate and PPh3, followed by stirring at 100° C. for 5 hours. After leaving to be cooled, a saturated aqueous NH4Cl solution was added thereto, followed by extraction with EtOAc. The organic layer was washed with brine, dried over MgSO4, and then concentrated under reduced pressure, followed by purification by silica gel column chromatography (hexane:EtOAc=95:5 to 80:20) to obtain methyl 5-isopropenyl-4-phenylthiophene-2-carboxylate as a colorless liquid.

WORKUP

后处理

  1. customAfter leaving
  2. temperatureto be cooled
  3. extractionfollowed by extraction with EtOAc
  4. washThe organic layer was washed with brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated under reduced pressure
  7. customfollowed by purification by silica gel column chromatography (hexane:EtOAc=95:5 to 80:20)