Preparation method of snail killing agent crude medicine niclosamide
A technology of niclosamide and molluscicide, applied in the field of preparation of niclosamide as molluscicide in aquaculture and schistosomiasis departments, can solve the problems of refractory degradation, toxicity, high production cost, etc., and achieve product yield and the effect of improved purity, mild reaction conditions, and shortened reaction time
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Embodiment 1
[0024] 100.0 grams of 5-chlorosalicylic acid, 118.0 grams of 2-chloro-4-nitroaniline and 1.8 liters of solvent xylene were added in a 3000ml four-necked flask equipped with an electric stirrer, a thermometer, a reflux device and a dropping funnel. Add the composite catalyst solution that 14.0 grams of phosphorus trichloride, 8.0 grams of pyridine and 200ml xylenes form in the dropping funnel; Stir, oil bath is heated to 115 ℃, slowly add composite catalyst solution, constant temperature reaction 2.5 hours; After cooling crystallization, Suction filtration, collect the precipitate, the solvent xylene is recycled after treatment, the precipitate is washed 2 to 3 times with 100ml of water, and then washed 2 to 3 times with 50ml of a composite organic solvent composed of acetone and ethanol with a mass ratio of 2.5:1 , and dried at 105°C to obtain 174.1 grams of light yellow crystalline powder product. According to high-pressure liquid chromatography analysis, the crystals contain...
Embodiment 2
[0026] The operation was the same as in Example 1, except that the raw material 2-chloro-4-nitroaniline was 92.0 grams, and the mass ratio of the composite organic solvent acetone and ethanol for washing the reaction product was 2.0:1. The obtained pale yellow crystalline powder product was 135.4 g. According to high-pressure liquid chromatography analysis, the crystals contain 90.3% of niclosamide. The calculated reaction yield was 70.1%.
Embodiment 3
[0028] The operation was the same as in Example 1, except that the composition of the composite catalyst solution was 17.0 grams of phosphorus pentachloride, 8.0 grams of pyridine and 200 ml of xylene. The resulting light yellow crystalline powder product was 171.6 g. According to high-pressure liquid chromatography analysis, the crystals contain 94.4% of niclosamide. The calculated reaction yield was 85.5%.
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