反应详情

温度

20 °C

In a glass-lined reactor 17.7 kg (3R,3aS,6aR)-hexahydrofuro[2,3-b]furan-3-ol in acetonitrile (30%) was added, then 3.9 kg of triethylamine 9 kg of solid disuccinimidyl carbonate (DSC) was added in portions, while keeping the reaction temperature below 35° C. The reaction mixture was stirred at 20° C. for 3 hours. The temperature was lowered to 2° C. and 45 kg of ice-water was added to the reactor. Precipitation was observed and the precipitate was filtered off. The cake was dissolved in 41 kg of chloroform and the aqueous phase was separated. The solution was evaporated to dryness and 18.8 kg of petroleum ether was added to the reactor containing the residue. The mixture was stirred at 0-5° C. for 1 hour. The resulting white precipitation was filtered off and rinsed with about 2 kg of petroleum ether. 1-([[(3R,3aS,6aR)hexahydrofuro[2,3-b]furan-3-yloxy]carbonyl]oxy)-2,5-pyrrolidinedione was obtained as an off-white solid, weight 3.69 kg (yield 39.9%, purity 68.7% by HPLC area, mobile phase: CH3CN/15 mmol/L Na2HPO4, pH 3.0 by H3PO4(35/65); speed: 0.8 mL/min; retention time: 7.730 min.).

1. customthe reaction temperature below 35° C
2. customwas lowered to 2° C.
3. customPrecipitation
4. filtrationthe precipitate was filtered off
5. dissolutionThe cake was dissolved in 41 kg of chloroform
6. customthe aqueous phase was separated
7. customThe solution was evaporated to dryness and 18.8 kg of petroleum ether
8. additionwas added to the reactor
9. additioncontaining the residue
10. stirringThe mixture was stirred at 0-5° C. for 1 hour
11. customThe resulting white precipitation
12. filtrationwas filtered off
13. washrinsed with about 2 kg of petroleum ether