HRID2294147
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
PROCEDURE
实验过程
A mixture of 2-amino-N,N-dimethylbenzamide (1.15 g, 6,97 mmol), prepared as in Example 22, potassium carbonate (1.44 g, 10.46 mmol) and 1-bromo-3-chloro-propane (0.7 mL, 7 mmol) in 10 mL of DMF was stirred at room temperature for 16 hours and then at 70° C. for an additional 4 hours. The mixture was poured into water and extracted with ethyl acetate (3×20 mL). The combined extract was washed with brine, dried (MgSO4) and concentrated to give 2-(3-chloropropyl)amino-N,N-dimethylbenzamide as a crude mixture.
WORKUP
后处理
- waitat 70° C. for an additional 4 hours
- extractionextracted with ethyl acetate (3×20 mL)
- extractionThe combined extract
- washwas washed with brine
- dry with materialdried (MgSO4)
- concentrationconcentrated