Methanol → Fluconazole

関与物質

反応手順

A mixture of 7.5 g (0.02 mol) of 2-(2,4-difluorophenyl)-1,3-bis(1,2,4-triazole-1-yl)-2-(trimethylsilyloxy)propane, 40 ml of methanol, 3 ml of water and 0.1 g of sodium hydroxide was stirred at room temperature for 1 h. After adding 300 ml of water the solution was concentrated to a volume of 50 ml with vacuum distillation. The obtained suspension was cooled to 0° C. and filtered. The obtained product was 6.12 g, water content was 11.5%. This was placed into a 100 ml flask and 0.1 g of crystal modification I of fluconazole seeding crystals were added thereto. The compound was dried on rotary evaporator at 80° C. for 3–4 h, until the weight was constant. 5.45 g of title compound was obtained. Yield: 87.4%. Mp.: 139–141° C.

情報源と証拠