反应详情

温度

100 °C

A mixture of 1,5,5 trimethylhydantoin (7.0 g, 49.2 mmol), powdered potassium carbonate (8.16 g, 59 mmol) and 2-methoxymethyloxy-allyl chloride (7.65 g, 56 mmol) in dry DMF (100 mL) was heated to 100° C. with stirring for 1.5 h. The reaction mixture was cooled, fliltered and the filtrate was concentrated, then partitioned between ethyl acetate and water. The organic extract was washed twice with water, brine, dried and concentrated, then purified via silica gel chromatography eluting with 50% ethyl acetate: hexane to give 10.58 g (89%) of the title compound.

1. temperatureThe reaction mixture was cooled
2. concentrationthe filtrate was concentrated
3. custompartitioned between ethyl acetate and water
4. extractionThe organic extract
5. washwas washed twice with water, brine
6. customdried
7. concentrationconcentrated
8. custompurified via silica gel chromatography
9. washeluting with 50% ethyl acetate