HRID270654

反应详情

EQUATION

反应方程式

HRID 270654 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

10.0 g of 2-thiopheneethanol, 11.5 g of 1,3-dioxolane, and 862 mg of indium(III) chloride were added to 780 mL of acetonitrile, and the resulting mixture was refluxed for 10 hours. The reaction product solution was cooled to room temperature and concentrated by evaporation under reduced pressure. To the residue, 100 mL of water and 150 mL of n-hexane were added, and the resulting mixture was stirred for 5 minutes. The organic layer was separated and dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was distilled under reduced pressure to obtain 6.6 g (yield of 60%) of the title compound, of which analysis data were the same as obtained in Example 14.

WORKUP

后处理

  1. temperaturethe resulting mixture was refluxed for 10 hours
  2. concentrationconcentrated by evaporation under reduced pressure
  3. additionTo the residue, 100 mL of water and 150 mL of n-hexane were added
  4. customThe organic layer was separated
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. distillationThe residue was distilled under reduced pressure