HRID1414375

反应详情

EQUATION

反应方程式

HRID 1414375 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution containing 4.8 g (87.6 mmole) of KOH dissolved in 200 ml of water was added 10 g (29.2 mmole) of 2-[p-carbomethoxyphenyl]-5,6-dinitrobenzimidazole (as prepared in (a) above). The resulting mixture was heated at 90° C under nitrogen for 8 hours, at which time it was allowed to cool to room temperature. The solution was then slowly acidified with 50% HCl, liberating the dinitro-acid as a light-tan precipitate. The product was collected by filtration, washed with several portions of distilled water and air-dried. Recrystallization from THF-heptane afforded golden platelets, m.p.--dec. above 350° C.

WORKUP

后处理

  1. temperatureto cool to room temperature
  2. filtrationThe product was collected by filtration
  3. washwashed with several portions of distilled water
  4. customair-dried
  5. customRecrystallization from THF-heptane afforded golden platelets, m.p.
  6. customabove 350° C.