4-Methylmorpholine → HCID 21218514, compound

Participants

Reaction Steps

7 g (11 mmol) of a 50% strength solution of propanephosphonic anhydride in dichloromethane are added to a solution of 2.8 g (10 mmol) of 2-(3-nitrophenylthio)-6-pyrazinecarboxylic acid, 3.2 g (25 mmol) of 2,4-difluoroaniline and 3 g (30 mmol) of 4-methylmorpholine in dichloromethane at 0° C. The reaction mixture is heated to room temperature. After 12 hours, the solvent is istilled off under reduced pressure. The residue is taken up in diethyl ether and the solution is extracted with 10% strength, aqueous hydrochloric acid, washed with distilled water and with saturated, aqueous sodium bicarbonate solution, dried over magnesium sulfate, filtered and freed from the solvent under reduced pressure. The crude product is purified by chromatography (silica gel, cyclohexane/ethyl acetate 4/1 (v/v)). Yield 1.6 g (40%); light yellow, crystalline solid, mp. 131-135° C.

Provenance & Evidence