反应详情

温度

97.5 °C

(2S,6R)-4-(2,4-Dimethoxy-benzyl)-2,6-dimethyl-3-oxo-piperazine-1-carboxylic acid benzyl ester (1.13 g, 2.74 mmol) is dissolved in 20 mL of acetonitrile. An aqueous solution of potassium persulfate (2.2 g, 8.23 mmol) and sodium phosphate (2.3 g, 16.5 mmol) in 12 mL of H2O is added, and the resulting mixture is heated to 95-100° C. for two hours. After cooling to room temperature, ethyl acetate (200 mL) is used to extract the aqueous layer and dried over magnesium sulfate. The residue after filtration and concentration is chromatographed (SiO2, 60% ethyl acetate/hexane) to give (2S, 6R)-2,6-Dimethyl-3-oxo-piperazine-1-carboxylic acid benzyl ester (480 mg, 67% yield) as a yellow oil.

1. temperatureAfter cooling to room temperature
2. extractionto extract the aqueous layer
3. dry with materialdried over magnesium sulfate
4. filtrationThe residue after filtration and concentration
5. customis chromatographed (SiO2, 60% ethyl acetate/hexane)