反应 #1605772
ord-684e4b93eb264e9eb912c3a906b4b0a4
反应方程式
NH3
2-methoxy-4-methylbenzoic acid
EDC
HOBt
→
2-methoxy-4-methylbenzamide
收率 83.0%
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1洗涤then washed successively with HCl (1N)
- 2干燥NaHCO3, water and brine, dried over MgSO4
- 3过滤filtered
- 4其他evaporated
- 5其他The residue was recrystallized from ethyl acetate/hexane
实验过程
To a mixture of 2-methoxy-4-methylbenzoic acid (20 g, 120.4 mmol), EDC (23.1 g, 120.4 mmol) and HOBt (16.3 g, 120.4 mmol) in dichloromethane (1 L) was added NH3 (7N in MeOH, 52 mL, 3 eq) dropwise. The reaction mixture was stirred at room temperature overnight then washed successively with HCl (1N), saturated aq.NaHCO3, water and brine, dried over MgSO4, filtered and evaporated. The residue was recrystallized from ethyl acetate/hexane to give 16.5 gr of 2-methoxy-4-methylbenzamide (83% yield).