反应详情

To a stirred solution of 5,5-dimethylhydantoin (10 g, 78 mmole) in methyl ethyl ketone (500 mL) at room temperature was added potassium carbonate (13 g, 94.1 mmole), followed by propargyl bromide (14 g, 80% in toluene, 94.1 mmole). The reaction mixture was then refluxed for 2.5 hr. The mixture was cooled to room temperature and the solid was filtered by suction filtration. The filtrate was concentrated on a rotary evaporator to give 12.5 g (96%) of 3-(2-propynyl)-5,5-dimethylhydantoin as a yellow solid, mp=156°-160° C. An NMR spectrum showed the desired product with a purity about 95%. This intermediate was subjected to the next step without further purification.

1. temperatureThe reaction mixture was then refluxed for 2.5 hr
2. filtrationthe solid was filtered by suction filtration
3. concentrationThe filtrate was concentrated on a rotary evaporator