反应详情

温度

0 °C

To a solution of 2 g of 1-benzoylisonipecotic acid (Step A) in 50 mL THF at 0° C. were added 1.47 g of triethylamine and 1.99 g of isobutyl chloroformate. The reaction was stirred for 1 h at 0° C. To a solution of 1.10 g of sodium borohydride in 30 mL DMF at 0° C. was slowly added the above THF mixture. The reaction was again stirred for 1 h at 0° C. Water (80 mL) was slowly added to the reaction and the mixture was extracted 5×80 mL ethyl acetate and the combined organic layers were dried over magnesium sulfate. The solvent was then evaporated under reduced pressure. The residue was purified by flash chromatography with 1:1 hexane : ethyl acetate followed by hexane : ethyl acetate: methanol, 50:50:5 to give 1.865 g of the title compound.

1. stirringThe reaction was again stirred for 1 h at 0° C
2. extractionthe mixture was extracted 5×80 mL ethyl acetate
3. dry with materialthe combined organic layers were dried over magnesium sulfate
4. customThe solvent was then evaporated under reduced pressure
5. customThe residue was purified by flash chromatography with 1:1 hexane