Synthesis method of tetramisole hydrochloride
A technology of tetraimidazole hydrochloride and a synthesis method, which is applied in the field of veterinary medicine and pharmaceutical raw material synthesis, can solve the problems of many impurities, cumbersome technological process, low yield and the like, and achieves the effects of simplifying the technological process, shortening the synthesis route and improving the prospect of industrialization.
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[0027] A kind of synthetic method of tetramisole hydrochloride is characterized in that taking (S)-3-(2-hydroxyl-2-phenylethyl)-2-iminothiazolidinone hydrochloride as reaction raw material to synthesize tetramisole, And by one step tetramisole is acidified into salt with hydrochloric acid and synthesizes hydrochloric acid, comprises the following steps:
[0028] Step (1): (S)-3-(2-hydroxy-2-phenylethyl)-2-iminothiazolidinone hydrochloride uses hydrochloric acid as a solvent, adds chlorosulfonic acid to the system, adjusts alkali and filters to obtain Tetramisole free base;
[0029] Step (2): add hydrochloric acid to the aqueous solution for tetramisole free base to acidify, and obtain tetramisole hydrochloride product after distillation and crystallization.
[0030] In the step (1), the mass ratio of chlorosulfonic acid to (S)-3-(2-hydroxyl-2-phenylethyl)-2-iminothiazolidinone hydrochloride is (0.45-0.92): 1 .
[0031] In the step (1), the mass ratio of hydrochloric acid to...
Embodiment 1
[0035] This embodiment provides a synthetic method of tetramisole hydrochloride, comprising the following steps: taking 25.850 g of (S)-3-(2-hydroxy-2-phenylethyl)-2-iminothiazolidinone hydrochloride and adding Add 25.850g of hydrochloric acid with a content of 36.50% to a four-necked bottle with mechanical stirring, control the temperature in the water bath at 45°C to 50°C, slowly add 17.50g of chlorosulfonic acid dropwise under stirring, and strictly control the reaction temperature at 45°C during the dropwise addition. ℃~50℃, after adding, cool the ice water to about 10℃, then slowly adjust the pH to 9.5~10.5 with a NaOH aqueous solution with a mass percentage concentration of 35%, and filter to obtain 20.40 g of tetramisole free base after the pH value is stable. The yield is 98.50%, and the purity is 98.62%.
[0036] Tetraimidazole free base is added into purified water with a four-fold mass ratio, acidified with hydrochloric acid at room temperature to form a salt, and t...
Embodiment 2
[0038] This embodiment provides a synthetic method of tetramisole hydrochloride, comprising the following steps: taking 25.850 g of (S)-3-(2-hydroxy-2-phenylethyl)-2-iminothiazolidinone hydrochloride and adding Add 12.60g of hydrochloric acid with a content of 36.50% to a four-necked bottle with mechanical stirring, control the temperature in a water bath at 45°C to 50°C, slowly add 17.50g of chlorosulfonic acid dropwise under stirring, and strictly control the reaction temperature at 45°C during the dropwise addition. ℃~50℃, after adding, cool the ice water to about 10℃, then slowly adjust the pH to 9.5~10.5 with a NaOH aqueous solution with a mass percentage concentration of 30%, and filter to obtain 20.10 g of tetramisole free base after the pH value is stable. The yield was 96.30% and the purity was 97.87%.
[0039] Tetraimidazole free base is added into purified water with a four-fold mass ratio, acidified with hydrochloric acid at room temperature to form a salt, and the...
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