反应详情

To a solution of 2.23 g (10.67 mmol) of 3-bromo4-oxo-pentanoic acid methyl ester in 11 mL of DMF at 0° C. was added 690 mg (10.67 mmol) of sodium azide. After warming to RT over 2.5 h, the reaction was diluted with water and extracted with diethyl ether/hexane (1:1). The layers were separated, the organics dried (Na2SO4), and the solvent removed in vacuo. The residue was purified by silica gel chromatography using diethyl ether/hexane (gradient of 1:4 to 2:3) to give 1.07 g (58% yield ) of the title compound: low resolution MS (FAB) m/e 172 (MH+).

1. extractionextracted with diethyl ether/hexane (1:1)
2. customThe layers were separated
3. dry with materialthe organics dried (Na2SO4)
4. customthe solvent removed in vacuo
5. customThe residue was purified by silica gel chromatography