反应详情

To a mixture of isoxazolidine hydrochloride (11.0 g) and chloroform (200 ml) was added (±)-2-chloropropionyl chloride (13.3 g) under ice-cooling and stirring and then added dropwise triethylamine (22.2 g) under the same conditions. The stirring was continued at room temperature for further one hour, after which an amount of water was added to the reaction mixture to form layers. The organic layer thus separated was washed with 1 N hydrochloric acid and then with a 5% aqueous sodium bicarbonate solution and dried over anhydrous sodium sulfate. Removal of the solvent by a distillation in vacuo gave N-[(±)-2-chloropropionyl]isoxazolidine (15.0 g) as a pale yellow oil. Purification of the oil by silica gel column chromatography afforded a colorless oil. nD20 =1.4918.

1. temperaturecooling
2. customto form layers
3. customThe organic layer thus separated
4. washwas washed with 1 N hydrochloric acid
5. dry with materialwith a 5% aqueous sodium bicarbonate solution and dried over anhydrous sodium sulfate
6. customRemoval of the solvent
7. distillationby a distillation in vacuo