实验操作An inert reactor was charged with 14 (87.4 kg, 1.00 equiv), 12 (59 kg, 1.05 equiv), MeCN (392 kg, 500 L), and NEt3 (29 kg, 1.5 equiv). A 50% T3P in DMF (183 kg, 1.5 equiv) was slowly charged maintaining an internal temperature of no more than 35 °C. The mixture was agitated at 20 °C for 3 h, and then DMF (87 kg, 92 L), water (218 kg), and 15 (0.26 kg) were charged. To the mixture was added water (392 kg) over no less than 2 h. The resulting slurry was aged for 2 h and then filtered. The filter cake was washed with a solution of water (392 kg) and MeCN (305 kg, 388 L), and then the solids were dried under vacuum at 50 °C to afford 15 as a white crystalline solid (129 kg, 91.5% yield, 100% purity by UPLC analysis)
