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温度

0 °C

To a solution of diester 58 (3.88 g, 20.2 mmol) in dry acetonitrile (40 mL) at 0° C., under Argon, was added slowly benzyl chloroformate (3.17 mL, 1.1 equiv.). The solution was stirred at 0° C. for 1 h after which it was poured into water (50 mL). The phases were separated and the aqueous layer was extracted with dichloromethane (3×50 mL). the combined organic extracts were washed with 5% HCl, water, brine and dried over anhydrous sodium sulfate. Evaporation of the solvents was followed by distillation to afford compound 70 as a colorless oil (5.4 g, 80%).

1. customThe phases were separated
2. extractionthe aqueous layer was extracted with dichloromethane (3×50 mL)
3. washthe combined organic extracts were washed with 5% HCl, water, brine
4. dry with materialdried over anhydrous sodium sulfate
5. customEvaporation of the solvents
6. distillationwas followed by distillation