反应详情

To a cold (0° C.) solution of 4-acetyl-5-[(1,1-dioxido-1,2-thiazinan-2-yl)methyl]-1-(4-fluorobenzyl)-piperazin-2-one (75 mg, 0.19 mmol) and diethyl oxalate (29 μL, 0.21 mmol) in DMF (3 mL) under an atmosphere of nitrogen, a solution of sodium bis(trimethylsilyl)amide in THF (1M, 0.21 mL, 0.21 mmol) was added over a period of 0.5 h and stirred at the temperature for 30 min. Then additional sodium bis(trimethylsilyl)amide in THF (1M, 0.21 mL, 0.21 mmol) was added over a period of 0.5 h and stirred at the temperature for 1 h. The product mixture was concentrated under vacuum, and the residue partitioned between aqueous HCl and ethyl acetate. The organic extract was dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum. The residue was subjected to HPLC purification on C-18 stationary phase eluted with water/acetonitrile/TFA mobile phase. Collection and lyophilization of appropriate fractions provided the title compound.

1. stirringstirred at the temperature for 1 h
2. concentrationThe product mixture was concentrated under vacuum
3. customthe residue partitioned between aqueous HCl and ethyl acetate
4. extractionThe organic extract
5. dry with materialwas dried over anhydrous magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated under vacuum
8. customThe residue was subjected to HPLC purification on C-18 stationary phase
9. washeluted with water/acetonitrile/TFA mobile phase
10. customCollection and lyophilization of appropriate fractions