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With potassium carbonate; In DMF (N,N-dimethyl-formamide); at 20℃; for 72h;
To a solid mixture of Example 273 Part A(2) compound (1.00 g, 2.35 mmoL), 2-methyl-5-nitroimidazole (400 mg, 3.15 mmol), and K2CO3 (2.82 mmol) was added DMF (5 mL) and the mixture was stirred at room temperature for 3 days. The reaction was partitioned between EtOAc and saturated NaHCO3 and the organic layer was washed successively with H2O and brine. The solution was dried (Na2SO4), filtered, and stripped. The residue was triturated with Et2O/EtOAc/hexane to give title compound (973 mg, 88%) as a white solid. mp 145-147C.
Preparation of crude tinidazole: 20Kg of beta-hydroxyethyl sulfide and 28Kg of 2-methyl-5-nitroimidazole were added to a 200L reaction kettle, then 45L of toluene was added, the temperature was increased, and the temperature was added at 45 C. 2Kg of aluminum trichloride, stir well, and then heat up to 95 ± 2 for 2.5 hours. After the heat preservation is completed, cool to room temperature, filter, take the organic layer, and apply the filtered solid to the next batch.Start stirring, add 100 g of sodium molybdate to the mixed solution of the organic layer water washing solution, heat up to 45-50 C, add 10 kg of hydrogen peroxide dropwise, and keep it for 1 hour. Cool and filter to obtain 36.0 Kg of crude tinidazole.The tinidazole fine product was obtained: the crude tinidazole was dissolved in 70% ethanol water twice the crude quality of tinidazole, and decolorized by adding 2.0% by weight of activated carbon of tinidazole for 30 minutes, and filtered while hot, the filtrate was cooled to crystallize, and filtered. Drying yielded 30.8 kg of tinidazole fines, with a total yield of 66.1% (based on beta-hydroxyethyl sulfide). The melting point was 127.3 127.8 , and the content of HPLC was 99.90%.
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