反应详情

温度

40 °C

Phthalimide (3 g) was dissolved in dry tetrahydrofuran (70 ml) and added dropwise at room temperature to a suspension of sodium hydride (539 mg) in tetrahydrofuran (15 ml). This was followed by heating at 40° C. for one hour, and then a solution of chloroacetone (1.99 g) dissolved in tetrahydrofuran (15 ml) was added dropwise. The mixture was then kept at the reflux temperature for 15 hours. After cooling, it was added to an ice/water mixture and extracted three times with ethyl acetate. The combined organic phases were washed once with saturated sodium chloride solution and then dried over magnesium sulfate. The solvent was removed in vacuo and the residue was chromatographed on silica gel (n-heptane/ethyl acetate 2:1). 2.9 g of the title compound were isolated.

1. additionwas added dropwise
2. temperatureAfter cooling
3. extractionextracted three times with ethyl acetate
4. washThe combined organic phases were washed once with saturated sodium chloride solution
5. dry with materialdried over magnesium sulfate
6. customThe solvent was removed in vacuo
7. customthe residue was chromatographed on silica gel (n-heptane/ethyl acetate 2:1)