반응 #1605772

반응 방정식

NH3

2-methoxy-4-methylbenzoic acid

EDC

HOBt

→

2-methoxy-4-methylbenzamide

수율 83.0%

용매

dichloromethane

반응 조건

후처리

1. 1
   세척then washed successively with HCl (1N)
2. 2
   건조NaHCO3, water and brine, dried over MgSO4
3. 3
   여과filtered
4. 4
   기타evaporated
5. 5
   기타The residue was recrystallized from ethyl acetate/hexane

실험 절차

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).

출처