Reaktion #1605772

Reaktionsgleichung

NH3

2-methoxy-4-methylbenzoic acid

EDC

HOBt

→

2-methoxy-4-methylbenzamide

Ausbeute 83.0%

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenthen washed successively with HCl (1N)
2. 2
   TrocknenNaHCO3, water and brine, dried over MgSO4
3. 3
   Filtrationfiltered
4. 4
   Sonstigeevaporated
5. 5
   SonstigeThe residue was recrystallized from ethyl acetate/hexane

Vorschrift

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).

Quelle