Reaktion #220322

Reaktionsgleichung

2-(Trifluoromethyl)benzoyl chloride

2-amino-nicotinic acid

water

→

2-(2-trifluoromethyl-phenyl)-pyrido[2,3-d][1,3]oxazin-4-one

Ausbeute 60.0%

Lösungsmittel

pyridine

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture is heated at 158 C for 30 min
2. 2
   FiltrationThe solid is collected by vacuum filtration
3. 3
   Waschenwashed with water and diethyl ether
4. 4
   SonstigeThe product is dried

Vorschrift

2-(Trifluoromethyl)benzoyl chloride (4.2 ml, 29.2 mmol) is added dropwise to a solution of 2-amino-nicotinic acid (2.04 g, 14.76 mmol) in 20 ml of pyridine. The reaction mixture is heated at 158 C for 30 min then cooled to room temperature. The reaction is poured into 200 ml of water and an oil forms which solidifies upon stirring. The solid is collected by vacuum filtration and washed with water and diethyl ether. The product is dried to give 2-(2-trifluoromethyl-phenyl)-pyrido[2,3-d][1,3]oxazin-4-one (2.56 g, 60% yield) which may be used in the next step without further purification.

Quelle