HRID1439558

反应详情

EQUATION

反应方程式

HRID 1439558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred and cooled suspension of 31 parts of α-hydroxy-p-tolyl 2-thienyl ketone in 160 parts of dry benzene are added dropwise 24 parts of thionyl chloride at 10° C. Upon completion, stirring is continued overnight at room temperature. The reaction mixture is evaporated and the residue is evaporated twice more from toluene. The latter residue is triturated in petroleumether. The product is filtered off and dissolved in 320 parts of ether. This solution is stirred with charcoal, filtered and the filtrate is evaporated. The residue is crystallized from ethanol at -20° C, yielding α-chloro-p-tolyl 2-thienyl ketone.

WORKUP

后处理

  1. temperaturecooled
  2. stirringUpon completion, stirring
  3. customThe reaction mixture is evaporated
  4. customthe residue is evaporated twice more from toluene
  5. customThe latter residue is triturated in petroleumether
  6. filtrationThe product is filtered off
  7. dissolutiondissolved in 320 parts of ether
  8. stirringThis solution is stirred with charcoal
  9. filtrationfiltered
  10. customthe filtrate is evaporated
  11. customThe residue is crystallized from ethanol at -20° C