反应详情

温度

60 °C

tert-Butyl (E)-(2S,3S)-2-[2-(tert-butyl-dimethyl-silanyloxy)-ethyl]-3-[(S)-2-(4-but-2-ynyloxy-phenyl)-1-ethoxycarbonyl-ethylcarbamoyl]-11-(2-heptyl-[1,3]dioxolan-2-yl)-2-hydroxy-undec-4-enoate (3.92 g, 4.49 mmol) was dissolved in acetonitrile (43 mL), and an aqueous solution of 0.5 M citric acid (19 mL, 9.50 mmol) was then added. The mixture was then stirred at 60° C. for 2.5 hours. The reaction solution was cooled to room temperature, and a mixture of a saturated aqueous solution (3.0 mL) of sodium chloride and water (60 mL) was then added. The solution was extracted three times with 20% ethyl acetate/n-hexane (32 mL). The organic layers were combined, then washed twice with a saturated aqueous solution (32 mL) of sodium chloride, dried over anhydrous sodium sulfate, and filtered. The solvent was then distilled off under reduced pressure to obtain 3.24 g (4.54 mmol, quant) of No. 5328627.

1. temperatureThe reaction solution was cooled to room temperature
2. additionwas then added
3. extractionThe solution was extracted three times with 20% ethyl acetate/n-hexane (32 mL)
4. washwashed twice with a saturated aqueous solution (32 mL) of sodium chloride
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationfiltered
7. distillationThe solvent was then distilled off under reduced pressure
8. customto obtain 3.24 g (4.54 mmol, quant) of No