反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 165 °C
PROCEDURE
实验过程
2-Chloro-1H-benzimidazole (10.0 g, 0.066 mol), pyrrolidine (18.5 g, 0.26 mol), and ethanol (100 mL) were combined. The resulting solution was heated at 160-170° C. for 6 hours and then the solvent was evaporated. The resulting residue was mixed with water. The mixture was made strongly acidic with hydrochloric acid and then made basic with ammonium hydroxide. The resulting solid was isolated by filtration, washed with water and then air dried to provide 11.8 g of crude product as a tan powder. This material was recrystallized from ethyl acetate/methanol to provide 4.9 g of 2-pyrrolidino-1H-benzimidazole. Analysis: Calculated for C11H13N3: % C, 70.56; % H, 7.00; % N, 22.44. Found: % C, 70.13; % H, 7.05; % N, 22.70.
WORKUP
后处理
- customthe solvent was evaporated
- additionThe resulting residue was mixed with water
- customThe resulting solid was isolated by filtration
- washwashed with water
- customair dried
- customto provide 11.8 g of crude product as a tan powder
- customThis material was recrystallized from ethyl acetate/methanol