HRID1164257

反应详情

EQUATION

反应方程式

HRID 1164257 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into 100 ml. of a 10% aqueous hydrochloric acid solution 1.5 g. of Sn powder are added at 0° to 10° C., followed by the addition of 10.8 g. (0.033 moles) of 2-[(methoxycarbonyl)amino]-1H-benzimidazol-5-sulfonic acid chloride hydrochloride. The reaction mixture is stirred at the same temperature for one hour. Thereafter 10 g. of Fe powder are added and it is stirred at 25° to 30° C. for 6 hours. The metals are dissolved and 2-[(methoxycarbonyl)amino]-1H-benzimidazole-5-thiol precipitates. The precipitate is filtered off, dissolved in a 10% aqueous potassium hydroxide solution and is subsequently reacted with 6 ml. of n-propyl bromide at 40° to 45° C.

WORKUP

后处理

  1. additionof Sn powder are added at 0° to 10° C.
  2. additionfollowed by the addition of 10.8 g
  3. stirringit is stirred at 25° to 30° C. for 6 hours
  4. dissolutionThe metals are dissolved
  5. custom2-[(methoxycarbonyl)amino]-1H-benzimidazole-5-thiol precipitates
  6. filtrationThe precipitate is filtered off
  7. dissolutiondissolved in a 10% aqueous potassium hydroxide solution
  8. customis subsequently reacted with 6 ml
  9. customat 40° to 45° C.