反应详情

温度

60 °C

To a stirred solution of 2,4-Di-tert-butyl-6-{4-[3-(4,5-dimethyl-4H-[1,2,4]triazol-3-ylsulfanyl)-propyl]-piperazin-1-yl}-pyrimidine (7.47 g, 16.8 mmol) in isopropanol (74.70 g) was added a H3PO4 solution in water (8.23 g H3PO4 (85%) in 28.89 g of water). The solution was heated to 60° C. and seeded with a slurry of the tetra-phosphate salt (143 mg) in isopropanol (1.41 g). The mixture was slowly cooled to 20° C. and isopropyl acetate (103.99 g) was charged. The solid was filtered off and washed (2×28 g) with a solution of isopropanol/isopropyl acetate (1:1). The solid was dried in a vacuum oven at 72° C. to afford 13.1 g (96.3% yield) of 2,4-di-tert-butyl-6-{4-[3-(4,5-dimethyl-4H-[1,2,4]triazol-3-ylsulfanyl)-propyl]-piperazin-1-yl}-pyrimidine tetra-phosphate salt as a white solid.

1. temperatureThe mixture was slowly cooled to 20° C.
2. filtrationThe solid was filtered off
3. washwashed (2×28 g) with a solution of isopropanol/isopropyl acetate (1:1)
4. customThe solid was dried in a vacuum oven at 72° C.