实验操作In a suitable reactor, purged with nitrogen, water (664 kg) and DMSO (2570 kg) were charged. The mixture was stirred and heated to 85−95 °C. Keeping the temperature below 95 °C, a solution of 10 (384.5 kg, 90%) in DMSO was added to the reactor in not less than 4 h. Carbon dioxide and isobutene were released. The reaction was stirred at 85−95 °C for at least 3 h.
The mixture was cooled to 20−30 °C, and maintaining the temperature below 35 °C, water (2306 kg) was charged. The suspension was centrifuged and washed with water (664 kg). The crude product was charged in the reactor. Methanol (609 kg) was added, and the mixture was refluxed (about 55 °C) until complete dissolution. The solution was then cooled to 0−5 °C and stirred for at least 1 h. The suspension was centrifuged and washed with 10% MeOH in water (376 kg). The product was dried under a vacuum at 40 °C (233 kg, 98.1% assay, 91% corrected assay yield, 99.6% HPLC purity).参考文献https://doi.org/10.1021/acs.oprd.3c00477
