反应详情

A solution of p-toluenesulfonyl azide (592 mg; 3 mmol) in 1 ml of acetonitrile was added at room temperature to a solution of 3-oxo-6-heptenoic acid methyl ester (468 mg; 3 mmol) and triethylamine (306 mg; 3 mmol) in 5 ml of acetonitrile. The mixture was stirred for about 2 hours and the solvent was distilled off under a reduced pressure and the product was dissolved in 50 ml of ether. The solution was washed with a 5% aqueous solution of potassium hydroxide until no color remained in the aqueous phase and was further washed with a saturated aqueous solution of sodium chloride. The ether solution was dried over anhydrous magnesium sulfate and was filtered and condensed under a reduced pressure to obtain 530 mg of 2-diazo-3-oxo-6-heptenoic acid methyl ester as a yellow oily product. The crude product can be purified by distillation under reduced pressure.

1. distillationthe solvent was distilled off under a reduced pressure
2. dissolutionthe product was dissolved in 50 ml of ether
3. washThe solution was washed with a 5% aqueous solution of potassium hydroxide until no color
4. washwas further washed with a saturated aqueous solution of sodium chloride
5. dry with materialThe ether solution was dried over anhydrous magnesium sulfate
6. filtrationwas filtered
7. customcondensed under a reduced pressure