Preparation method of triclabendazole sulfoxide
A technology of triclbendazole sulfoxide and triclbendazole, which is applied in the field of organic chemical synthesis, can solve the problems of high consumption, high price, large molecular weight and the like, and achieves the effect of safe operation
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Embodiment 1
[0022] Add 40g (0.11mol) of triclabendazole and 400ml of methanol into a 500ml reaction flask, stir and heat until the triclabendazole dissolves, the temperature drops to 20-25°C, and add 0.2g of vanadium pentoxide. Add 15.7g (0.138mol) of 30wt% hydrogen peroxide dropwise, the dropwise addition time is 30 minutes, the dropwise addition temperature is controlled at 20-25°C, and then keep warm at 20-25°C until crystallization occurs, then add 10.0g of sodium sulfite (0.080mol) , stirred for 30 minutes, added 100ml of water, cooled to 10-20°C, filtered to obtain the wet product triclabendazole sulfoxide.
[0023] Put the wet product triclabendazole sulfoxide into a 500ml reaction bottle, add 300ml acetone, heat to reflux, reflux for 30 minutes, cool down to 45~50°C and filter to remove the catalyst vanadium pentoxide. The filtrate was distilled to remove the solvent from acetone until white crystals precipitated, added 130ml of methanol, heated to reflux for 1 hour, cooled to 15~...
Embodiment 2
[0025] Add 20 g (0.055 mol) of triclobendazole and 200 ml of ethanol into a 500 ml reaction flask, stir and heat until the triclobendazole dissolves, cool down, and add 0.2 g of vanadium pentoxide. Add 7.3g (0.064mol) of 30% hydrogen peroxide dropwise, the dropwise addition time is 40 minutes, the dropwise addition temperature is controlled at 25-30°C, and then keep warm at 25-30°C until crystals are precipitated, then add 5.0g of sodium sulfite (0.040mol) , add 100ml of water, cool to 10~20°C and filter to obtain the wet product triclabendazole sulfoxide.
[0026] Put the wet product triclabendazole sulfoxide into a 500ml reaction bottle, add 300ml acetone, heat to reflux, reflux for 1h, cool down to 40-45°C and filter, distill acetone from the reaction solution, and stop the distillation when there is white material , add 65ml of methanol, heat up to reflux for 45 minutes, cool down to 15-25°C, filter, and dry at 90°C to obtain a dry weight of 14.2g of triclabendazole sulfon...
Embodiment 3
[0028] Add 20g (0.055mol) of triclabendazole and 200ml of formic acid into a 500ml reaction bottle, stir and heat until triclabendazole dissolves, cool down to 30-35°C, add 0.1g of vanadium pentoxide, drop 7.0g (0.07mol) of 30wt% hydrogen peroxide, the dropping time is 50 minutes, the dropping temperature is controlled at 30-35°C, and then kept at 30-35°C for 4 hours, add 5.0g of sodium sulfite (0.040mol), add 200ml water, cooled to 10-20°C and filtered to obtain the wet product triclabendazole sulfoxide.
[0029] Put the wet product triclabendazole sulfoxide into a 500ml reaction bottle, and add 300ml of acetone. Heat to reflux, reflux for 1h, cool down to 40-45°C and filter, distill acetone from the reaction solution, stop distillation when there is white material, add 65ml of 95% ethanol, heat up to reflux for 45 minutes, cool to 15-25°C and filter, 90°C Dried to obtain a dry weight of 12.9 g triclabendazole sulfoxide, HPLC purity 97.8%, of which 0.8% triclabendazole, 1.2%...
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