反应详情

A solution of 3-buten-1-ol (1 g, 13.9 mmol), triphenylphosphine (4.73 g, 18 mmol) and 5,5-dimethylhydantoin (2.1 g, 16.7 mmol) in THF (50 mL) was treated dropwise with diethylazodicarboxylate (3.13 g, 18.0 mmol), stirred at ambient temperature for 1 hour, treated with water and partitioned between ethyl acetate and brine. The organic layer was dried (Na2SO4), filtered, and concentrated to provide crude product which was purified on silica gel with 50% ethyl acetate/hexanes to provide 2.5 g (100%) of the title compound.

1. custompartitioned between ethyl acetate and brine
2. dry with materialThe organic layer was dried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated
5. customto provide crude product which
6. customwas purified on silica gel with 50% ethyl acetate/hexanes