反应详情

To a stirred solution of 3-(2-propynyl)-5,5-dimethylhydantoin (3 g, 18.1 mmole) in methyl ethyl ketone (125 mL) at room temperature was added K2CO3 (2.8 g, 20.3 mmole), followed by propargyl bromide (3 g, 80% in toluene, 20.2 mmole). The reaction mixture was then refluxed for 24 hr. The reaction mixture was cooled to room temperature and was diluted with water and extracted with methylene chloride (3×125 mL). The organic layer was washed with saturated NaCl and dried over MgSO4. Evaporation of the volatiles yielded 3.3 g (89 %) of 1,3-di-propargyl-5,5-dimethylhydantoin as a light yellow semi-solid. An NMR spectrum showed the desired structure. This intermediate was subjected to the next step without further purification.

1. temperatureThe reaction mixture was then refluxed for 24 hr
2. extractionextracted with methylene chloride (3×125 mL)
3. washThe organic layer was washed with saturated NaCl
4. dry with materialdried over MgSO4
5. customEvaporation of the volatiles