反应详情

Fuming nitric acid (1.5 ml, 36.2 mmol) was added slowly at 0° C. to a solution of 3-methoxy-4-(3-morpholinopropoxy)benzoic acid (7.78 g, 23.5 mmol) in TFA (25 ml). The cooling bath was removed and the reaction mixture stirred at ambient temperature for 1 hour. The TFA was removed by evaporation and ice was added to the residue. The precipitate was collected by filtration, washed with a minimum of water followed by toluene and ether. The solid was dried under vacuum over phosphorus pentoxide to give 5-methoxy-4-(3-morpholinopropoxy)-2-nitrobenzoic acid (7.54 g) which was used without flirther purification.

1. customThe cooling bath was removed
2. customThe TFA was removed by evaporation and ice
3. additionwas added to the residue
4. filtrationThe precipitate was collected by filtration
5. washwashed with a minimum of water
6. dry with materialThe solid was dried under vacuum over phosphorus pentoxide