反応 #1605772

反応方程式

NH3

2-methoxy-4-methylbenzoic acid

EDC

HOBt

→

2-methoxy-4-methylbenzamide

収率 83.0%

溶媒

dichloromethane

反応条件

後処理

1. 1
   洗浄then washed successively with HCl (1N)
2. 2
   乾燥NaHCO3, water and brine, dried over MgSO4
3. 3
   ろ過filtered
4. 4
   その他evaporated
5. 5
   その他The residue was recrystallized from ethyl acetate/hexane

実験手順

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).

出典