HRID9657

反应详情

EQUATION

反应方程式

HRID 9657 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of tributyl[5-(1,3-dioxolan-2-yl)4-methylthien-2-yl]stannane (intermediate 76, 2.92 g), 1M aqueous hydrochloric acid (3 ml) and tetrahydrofuran (10 ml) was stirred at reflux for 30 minutes. The reaction mixture was cooled, extracted thrice with diethylether. The organic solutions were combined, extracted with saturated sodium bicarbonate and dried with brine and over magnesium sulfate. The product isolated after evaporation of the solvent was further purified by flash column chromatography using cyclohexane:ethyl acetate (50:1) as eluent to give the title compound as a yellow oil.

WORKUP

后处理

  1. temperatureat reflux for 30 minutes
  2. temperatureThe reaction mixture was cooled
  3. extractionextracted thrice with diethylether
  4. extractionextracted with saturated sodium bicarbonate
  5. dry with materialdried with brine and over magnesium sulfate
  6. customThe product isolated
  7. customafter evaporation of the solvent
  8. customwas further purified by flash column chromatography