HRID1164928

反应详情

EQUATION

反应方程式

HRID 1164928 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Powdered anhydrous potassium carbonate (4.3 kg, 31 moles) was added to a mixture of 1,3-dibromopropane (6.55 kg, 32 moles), thiophenol (1.2 kg, 10.9 moles) and methylethylketone (9 L). The alkylation was carried out under a hood in a 22 liter flask equipped with a mechanical stirrer, heating mantle, and 2 reflux condensers. Nitrogen gas was passed over the top of the condensers. Within 30 minutes the mixture had generated enough heat to attain reflux. Reflux was then maintained for another 30 to 60 minutes. The mixture was permitted to come to room temperature over an 18 hour period. The solvent layer was siphoned off and filtered through celite. The salts were filtered and washed with acetone. The filtrates were concentrated. The residue was vacuum distilled. Three fractions were collected:

WORKUP

后处理

  1. customThe alkylation was carried out under a hood in a 22 liter flask
  2. customequipped with a mechanical stirrer
  3. temperatureheating mantle
  4. temperature2 reflux condensers
  5. temperatureWithin 30 minutes the mixture had generated enough heat
  6. temperatureto attain reflux
  7. temperatureReflux
  8. temperaturewas then maintained for another 30 to 60 minutes
  9. filtrationfiltered through celite
  10. filtrationThe salts were filtered
  11. washwashed with acetone
  12. concentrationThe filtrates were concentrated
  13. distillationdistilled
  14. customThree fractions were collected