|
|
24 liters of dimethylacetamide, 110 liters of acetone, and 24 kg of dimethyl-2-propylimidazole-4,5-dicarboxylate were taken into a reactor and stirred for 45minutes. 29.2 kg of potassium carbonate, and 62 kg of 5-[4-(bromomethyl)一[1,1-biphenyl]-2-y1]-2H-tetrazole were then added. Another 20 liters of acetone was used to rinse the walls of the reactor. The reaction mass was heated to 61 0C and maintained for 6 hours. Reaction completion was checked using thin layer chromatography. After the reaction was completed, about 70%of the acetone was distilled off atmospherically from the reaction mass at 61 0C. The reaction
mass was then cooled to 36 0C and 240 liters of water was added, and a vacuum of 680 mm Hg was applied to distill off the remaining acetone. The remaining reaction mass was filtered and the solid was washed with 60 liters of water. 152 liters of toluene was taken into a reactor and the wet solid obtained after filtration was added to it. The mixture was heated to 84 0C to get clear dissolution. After clear dissolution was obtained, the solution was cooled to 34 0C. The solution was maintained at that temperature for 1 hour for complete isolation of the solid. It was then filtered and the wet solid was washed with 38 liters of toluene. The wet material was dried under a vacuum of 600 mm Hg and a temperature of 70 0C for 5 hours. The dry material was milled and again dried at 77 0C under a vacuum of 600 mm Hg for 3 hours to yield 61.8 kg of the title compound. (Yield 82.8%).Purity by HPLC: 99.4%.
能不能帮忙翻一下这段啊 |
|