反应详情

温度

0 °C

A solution of EXAMPLE 350A (5.25 g) in tetrahydrofuran (40 mL) was added dropwise to a solution of lithium diisopropylamide (12 mL, 2.0M in tetrahydrofuran/heptane/ethylbenzene) at 0° C. The solution was stirred at 0° C. for 30 minutes, and then was transferred by cannula to a pre-cooled (0° C.) stirring solution of N-fluorobenzenesulfonimide (7.89 g) in dry tetrahydrofuran (20 mL). The reaction mixture was stirred at 0° C. for 30 minutes, and then at 20° C. for 18 hours. The reaction mixture was poured over aqueous NH4Cl and extracted with diethyl ether (3×200 mL). The combined organic layers were washed with water, brine and dried over Na2SO4. Filtration and evaporation of the solvent gave the crude product.

1. temperaturea pre-cooled (0° C.)
2. stirringThe reaction mixture was stirred at 0° C. for 30 minutes
3. waitat 20° C. for 18 hours
4. extractionextracted with diethyl ether (3×200 mL)
5. washThe combined organic layers were washed with water, brine
6. dry with materialdried over Na2SO4
7. filtrationFiltration and evaporation of the solvent