HRID3248

反应详情

EQUATION

反应方程式

HRID 3248 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Initially, 3 g of 8-bromomethylquinoline was added to a solution of 1 g of 5,5-dimethyl-2,4-dithiohydantoin in 50 mL of ethanol (EtOH). The reaction mixture was stirred at the room temperature for 1.5 hour, and concentrated in vacuo. To the residue, 100 mL of CHCl3 was added. The mixture was washed with an aqueous solution of K2CO3, dried over MgSO4 and concentrated in vacuo. The residue was purified by column chromatograph (CHCl3). Recrystallization from diethyl ether gave the desired compound in the form of a needle-like crystal. The yield of this compound was 2.3 g with a yield ratio of 83.3%, and the melting point was 101°-104° C.

WORKUP

后处理

  1. concentrationconcentrated in vacuo
  2. additionTo the residue, 100 mL of CHCl3 was added
  3. washThe mixture was washed with an aqueous solution of K2CO3
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by column chromatograph (CHCl3)
  7. customRecrystallization from diethyl ether