HRID462565

反应详情

EQUATION

反应方程式

HRID 462565 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a 100 ml reaction flask equipped with reflux condensor, heating mantle, hot plate equipped with magnetic stirring apparatus and magnetic stirring bar is placed 10 ml cyclohexane, 0.5 grams of para toluene sulfonic acid and 10.8 grams (0.1 mole) of 1,2-propanedithiol. Over a period of one hour, 9 grams (0.1 mole) of methylthioacetaldehyde is added to the reaction mass. The reaction mass is then heated to reflux and maintained at reflux for a period of eight hours. At the end of the eight hour period the reaction mass is transferred to a separatory funnel and washed with one 50 ml portion of a saturated aqueous sodium chloride solution, then dried over anhydrous sodium sulfate, filtered and distilled. The distillation takes place on a micro vigreux column yielding the following fractions:

WORKUP

后处理

  1. customInto a 100 ml reaction flask
  2. customequipped
  3. temperaturewith reflux condensor
  4. temperatureheating mantle
  5. customhot plate equipped with magnetic stirring apparatus and magnetic stirring bar
  6. temperatureThe reaction mass is then heated
  7. temperatureto reflux
  8. temperaturemaintained
  9. temperatureat reflux for a period of eight hours
  10. customAt the end of the eight hour period the reaction mass is transferred to a separatory funnel
  11. washwashed with one 50 ml portion of a saturated aqueous sodium chloride solution
  12. dry with materialdried over anhydrous sodium sulfate
  13. filtrationfiltered
  14. distillationdistilled
  15. distillationThe distillation
  16. customyielding the following fractions