案例方程式
实验操作
To a mixture of 6 (6.50 kg, 95.0% potency, 1.0 equiv, limiting reagent), sodium dihydrogen phosphate (3.79 kg, 1.5 equiv), and dimethyl sulfoxide (4.5 L, 3.0 equiv) in 2-MeTHF (91.0 L, 15 L/kg) and water (19.5 L, 3 L/kg) at 10 °C was added, in four portions (10 + 20 + 30 + 40%), a solution of sodium chlorite (4.77 kg, 2.0 equiv) in water (26.0 L, 4 L/kg).
The addition rate was controlled carefully, and the reaction mixture was held for at least 1 h after the addition of each portion to keep the internal temperature below 15 °C. After all the oxidant solution had been added, the reaction mixture was held for at least another 4 h until UPLC analysis showed the oxidation was complete.
Excess oxidant was quenched with a solution of sodium bisulfite (5.49 kg, 2.5 equiv) in water (19.5 L, 3 L/kg),keeping the internal temperature below 15 °C. The mixture was checked by peroxide strip test for any residual oxidant. The phases were split, and the organic phase was washed with 3 M sodium chloride solution (19.5 L, 3 L/kg).
对应合成路线
参考文献
https://doi.org/10.1021/acs.oprd.4c00177
