Method for preparing ponazuril serving as anticoccidiosis medicament
An anti-coccidian and drug technology, applied in the direction of organic chemistry, can solve the problems of unresolved safety, high toxicity, explosive, etc., and achieve the effect of improving safety, reducing environmental impact, and reducing environmental pollution
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Embodiment 1
[0070] 1) Preparation of 3-methyl-4-(4-trifluoromethylthiophenoxy)-nitrobenzene (compound 1):
[0071] Weigh 200g (1.04mol) of 4-trifluoromethylthiophenol, DMF (200ml), 46g (1.06mol) of sodium hydroxide, heat to 90°C, add 176g (1.02mol) of 2-methyl-4-nitro The DMF (200ml) solution of chlorobenzene was heated to 140°C and reacted for 6 hours. The DMF was distilled off under reduced pressure, stirred and cooled to below 10°C, and a precipitate was precipitated, filtered with suction, washed with water, and dried to obtain 300.2 g of an orange-yellow solid. Yield: 93.4%. mp: 61°C to 62°C.
[0072] 2) Preparation of 3-methyl-4-(4-trifluoromethylthiophenoxy)-aniline (compound 2):
[0073] Weigh 300g (0.9mol) of 3-methyl-4-(4-trifluoromethylthiophenoxy)-nitrobenzene, 30g of activated carbon, and 15g of ferric chloride hydrate into the reaction flask, add 3L of 90% ethanol , heated to 80°C, added 150ml of 80% hydrazine hydrate, and reacted for 4 hours after the addition was comple...
Embodiment 2
[0081] 1) Preparation of 3-methyl-4-(4-trifluoromethylthiophenoxy)-nitrobenzene (compound 1):
[0082] Weigh 200g (1.04mol) of 4-trifluoromethylthiophenol, DMSO (200ml), 46g (1.06mol) of sodium hydroxide, heat to 90°C, add 176g (1.02mol) of 2-methyl-4-nitro Chlorobenzene in DMSO (200ml) solution, heated up to 140°C, reacted for 6 hours, distilled off DMF under reduced pressure, stirred and cooled to below 10°C, precipitated, filtered with suction, washed with water, dried to obtain 300g of orange solid, yield: 93.3 %. mp: 61°C to 62°C.
[0083] 2) Preparation of 3-methyl-4-(4-trifluoromethylthiophenoxy)-aniline (compound 2): Weigh 300g (0.9mol) 3-methyl-4-(4-trifluoromethyl Add thiophenoxy)-nitrobenzene, 15g of activated carbon, and 12g of ferric chloride hydrate into the reaction flask, add 3L of 90% ethanol, heat to 80°C, add 150ml of 80% hydrazine hydrate, and react for 4 hours after the addition. After the reaction was completed, the catalyst was removed by filtration, ...
Embodiment 3
[0088] 1) Preparation of 3-methyl-4-(4-trifluoromethylthiophenoxy)-nitrobenzene (compound 1):
[0089] Weigh 200g (1.04mol) of 4-trifluoromethylthiophenol, DMF (200ml), 146g (1.06mol) of potassium carbonate, heat to 90°C, add 176g (1.02mol) of 2-methyl-4-nitrochloride Benzene in DMF (200ml) solution, heated to 140°C, reacted for 6 hours, distilled off the DMF under reduced pressure, stirred and cooled to below 10°C, precipitated, filtered with suction, washed with water, and dried to obtain an orange-yellow solid.
[0090] 2) Preparation of 3-methyl-4-(4-trifluoromethylthiophenoxy)-aniline (compound 2): Weigh 300g (0.9mol) 3-methyl-4-(4-trifluoromethyl Add thiophenoxy)-nitrobenzene, 25g of activated carbon, and 18g of ferric chloride hydrate into the reaction flask, add 3L of 90% ethanol, heat to 80°C, add 150ml of 80% hydrazine hydrate, and react for 4 hours after the addition. After the reaction was completed, the catalyst was removed by filtration, the filtrate was concent...
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