HRID276048

反应详情

EQUATION

反应方程式

HRID 276048 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Oxalyl chloride (0.437 g) was added to a solution of 0.490 g of 6-carboxy-1-(2,4-dichlorobenzyl)-2-methylbenzimidazole and 1 drop of N,N-dimethylformamide in 8 ml of methylene chloride while being cooled with ice, and the mixture was stirred at room temperature for 1.5 hours. Four milliliters of 28% aqueous ammonia were added thereto, and the solution was stirred at room temperature for 12 hours. The reaction solution was extracted with the addition of water and methylene chloride. The organic layer was concentrated, and the crystals precipitated were then collected, and were dried to give 0.240 g of 6-carbamoyl-1-(2,4-dichlorobenzyl)-2-methylbenzimidazole (223).

WORKUP

后处理

  1. temperaturewhile being cooled with ice
  2. stirringthe solution was stirred at room temperature for 12 hours
  3. extractionThe reaction solution was extracted with the addition of water and methylene chloride
  4. concentrationThe organic layer was concentrated
  5. customthe crystals precipitated
  6. customwere then collected
  7. customwere dried