HRID2112824

反应详情

EQUATION

反应方程式

HRID 2112824 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A suspension of 1 g (3.6 mmol) of 2,5-dibromo-1H-benzimidazole and 0.85 mL (10.18 mmol) of pyrrolidine in 45 mL of acetonitrile is heated for 2 hours at 150° C. in the microwave. The reaction mixture is poured onto water and extracted with EtOAc. The organic phase is washed three times with water and dried over sodium sulfate. The solvent is distilled off, and the residue is stirred with DIPE and the solid is filtered off. Yield: 0.43 g (45% of theoretical); C11H12BrN3 (M=266.13); calc.: molpeak (M−H)—: 264/266; found: molpeak (M−H)−: 264/266; Rf value: 0.5 (silica gel, DCM/MeOH 10:1).

WORKUP

后处理

  1. additionThe reaction mixture is poured onto water
  2. extractionextracted with EtOAc
  3. washThe organic phase is washed three times with water
  4. dry with materialdried over sodium sulfate
  5. distillationThe solvent is distilled off
  6. filtrationthe solid is filtered off