反应详情

温度

0 °C

4-N-(t-Butyloxycarbonyl)-1,1-dioxo-6-hydroxy -2,3,4,5,6,7-hexahydro-1,4-thiazepine (10.0 g, 37.7 mmole) from Example 5, was dissolved in 110 mL of acetone, cooled to 0° C. and treated with 18.8 mL of freshly prepared Jones reagent. The reaction was stirred at ambient temperature for three hours and then treated with 5 mL of methanol. After 15 minutes, the reaction was filtered through magnesium sulfate and the filtrate immediately concentrated. The residue was filtered through a pad of silica gel using 3:1 chloroform-ethyl acetate to obtain the produce (9.67 g, 87%) D.C.I.M.S. 264(M+H) M.P. 172°-173° C.

1. waitAfter 15 minutes
2. filtrationthe reaction was filtered through magnesium sulfate
3. concentrationthe filtrate immediately concentrated
4. filtrationThe residue was filtered through a pad of silica gel using 3:1 chloroform-ethyl acetate
5. customto obtain the
6. customproduce (9.67 g, 87%) D.C.I.M.S