HRID1601709

反应详情

EQUATION

反应方程式

HRID 1601709 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

In 200 ml of N,N-dimethylacetamide (DMAC) were dissolved 31.0 g (0.166 mol) of 2-n-butyl-4-chloro-5-formylimidazole and 41.5 g (0.166 mol) of p-bromobenzyl bromide. After this solution was cooled to -10° C., 23.7 g (0.168 mol) of potassium carbonate particles which had a specific surface area of 1.5 m2 /g and in which the content of particles each having a diameter of 74 μm or smaller was 30% by weight were added to the solution over 10 minutes while holding the solution at -10 to -5° C. The resultant mixture was stirred at -10° C. for 2 hours, subsequently heated to room temperature, and then stirred for 2 hours to complete the reaction (which was conducted in an air atmosphere). Thereafter, the reaction mixture was filtered and the filtrate was cooled to 0° C. Thereto was added 320 ml of 15° C. water. The crystals thus precipitated were taken out by filtration to obtain 55.8 g of 2-n-butyl-4-chloro-1-(4-bromobenzyl)-5-formylimidazole having a purity of 99.8% (yield, 98.0%).

WORKUP

后处理

  1. additionwere added to the solution over 10 minutes
  2. customat -10 to -5° C
  3. temperaturesubsequently heated to room temperature
  4. customthe reaction (which
  5. filtrationThereafter, the reaction mixture was filtered
  6. temperaturethe filtrate was cooled to 0° C
  7. additionThereto was added 320 ml of 15° C. water
  8. customThe crystals thus precipitated
  9. filtrationwere taken out by filtration