HRID53504

反应详情

EQUATION

反应方程式

HRID 53504 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8.06 g of N-phenylpyrrolidinone were dissolved in 33 ml glacial acetic acid; the mixture was cooled to 0°-5° C. and then a solution of 2.65 ml bromine in 12 ml of glacial acetic acid was added dropwise. Stirring was continued for 30 minutes at room temperature. Work-up was accomplished by pouring the mixture into 1 l of water and neutralizing the mixture with KOH. The solid was filtered and dissolved in ethylacetate and washed with a sodium thiosulphate solution until the brown colour disappeared; washing with brine and drying with MgSO4 provided 8.5 g of a white crystalline mass that could be recrystallized from ether; m.p. 102° C.

WORKUP

后处理

  1. temperaturethe mixture was cooled to 0°-5° C.
  2. filtrationThe solid was filtered
  3. dissolutiondissolved in ethylacetate
  4. washwashed with a sodium thiosulphate solution until the brown colour
  5. washwashing with brine
  6. dry with materialdrying with MgSO4
  7. customprovided 8.5 g of a white crystalline mass that
  8. customcould be recrystallized from ether