反应详情

温度

20 °C

A mixture of 0.362 mol of 1-benzhydryl-3-mesyloxyazetidine (J. Org. chem. 1972, 37, 3953-3955), 0.44 mol of potassium phthalimide and 0.045 mol of hexadecyltributylphosphonium bromide in 500 ml of anhydrous toluene is heated at reflux for 5 hours, then it is cooled at 20° C. The precipitate is filtered, washed with 400 ml of ethyl acetate and discarded. The organic solution is washed with water, dried on anhydrous sodium sulfate, filtered on charcoal and concentrated under reduced pressure. The oily residue is crystallized from 600 ml of diisopropyl ether. Thus, 80 g (Yield: 67.4% of the theoretic) of 1-benzhydryl-3-phthalimidoazetidine are obtained; m.p. 118°-120° C.

1. temperatureis heated
2. temperatureat reflux for 5 hours
3. filtrationThe precipitate is filtered
4. washwashed with 400 ml of ethyl acetate
5. washThe organic solution is washed with water
6. dry with materialdried on anhydrous sodium sulfate
7. filtrationfiltered on charcoal
8. concentrationconcentrated under reduced pressure
9. customThe oily residue is crystallized from 600 ml of diisopropyl ether