تفاعل #1605772

معادلة التفاعل

NH3

2-methoxy-4-methylbenzoic acid

EDC

HOBt

→

2-methoxy-4-methylbenzamide

المردود 83.0%

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   غسيلthen washed successively with HCl (1N)
2. 2
   تجفيفNaHCO3, water and brine, dried over MgSO4
3. 3
   ترشيحfiltered
4. 4
   أخرىevaporated
5. 5
   أخرىThe residue was recrystallized from ethyl acetate/hexane

الإجراء التجريبي

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).

المصدر