HRID1494673

反应详情

EQUATION

反应方程式

HRID 1494673 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 1-(hex-5-ynyl)-4-n-propyl-2,6,7-trithiabicyclo[2.2.2]octane-2-oxide (0.302 g.) in dry acetone (120 ml) containing anhydrous magnesium sulphate (0.75 g) at -20° C. was added a solution of potassium permanganate (0.24 g) in dry acetone (25 ml). The mixture was allowed to warm to 20° and stirred for 72 hours. The colourless mixture was filtered through kieselguhr and the solid residue was washed with acetone. The filtrates were evaporated in vacuo and a colourless solid residue was obtained. The residue was purified by chromatography on silica eluting with dichloromethane. 1-(Hex-5-ynyl)-4-n-propyl-2,6,7-trithiabicyclo[2.2.2]octane-2,2-dioxide was obtained as a colourless solid (100 mg).

WORKUP

后处理

  1. temperatureto warm to 20°
  2. filtrationThe colourless mixture was filtered through kieselguhr
  3. washthe solid residue was washed with acetone
  4. customThe filtrates were evaporated in vacuo
  5. customa colourless solid residue was obtained
  6. customThe residue was purified by chromatography on silica eluting with dichloromethane