HRID9111

反应详情

EQUATION

反应方程式

HRID 9111 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

General Procedure for 1-(6-bromo-7-alkoxy-2-benzothiazolyl)-3-ethyl-urea compounds 9–13. A mixture of 1-(6-bromo-7-hydroxy-2-benzothiazolyl)-3-ethyl-urea 6 and potassium carbonate (1.05 eq) in anhydrous DMF was stirred at about 20° C. for about 0.5 hour, and was cooled down to about 0° C. The mixture was treated with an alkyl halide (1.0 eq), and was stirred at about 0–85° C. for about 16 hours. To the reaction mixture was added methanol. The solid was filtered off and washed with methanol. The solvent was evaporated and the residue was dissolved in DMF. The crude reaction solution was purified by preparature LC/MS to give pure desired product.

WORKUP

后处理

  1. temperaturewas cooled down to about 0° C
  2. stirringwas stirred at about 0–85° C. for about 16 hours
  3. filtrationThe solid was filtered off
  4. washwashed with methanol
  5. customThe solvent was evaporated
  6. dissolutionthe residue was dissolved in DMF
  7. customThe crude reaction solution
  8. customwas purified by preparature LC/MS