Preparation method of clopidogrel hydrogen sulfate and its intermediate n-(2-thienyl ethyl) methyleneamine
A technology of clopidogrel hydrogen sulfate and thiophene ethyl is applied in the field of medicine, and can solve the problems of great influence on the pulping yield of absolute ethanol, difficulty in concentrating dichloroethane, complicated experimental process, etc., so as to save time and cost of raw materials, Save time and cost of raw materials, the effect of simple process
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Embodiment 1
[0048]This embodiment provides a method for synthesizing N-(2-thiopheneethyl)methyleneamine, and the N-(2-thiopheneethyl)methyleneamine is prepared by the following method: adding 100.00 ml of a 250ml three-necked flask to a g 2-thiopheneethylamine, at the same time add 50.00g absolute ethanol (water content 0.34%) and 23.62g paraformaldehyde, under stirring, heat to 49-53 ℃, keep the temperature for 3h, then suction filtration while hot, the reaction system Naturally cooled to 38°C, white solid was precipitated, then continued to cool to 5-10°C, kept for 2h, suction filtered, and beaten with solvent (0.5 times the mass, temperature 5-10°C) to obtain white solid, which was placed in a blast drying oven (T= 40°C) and dried to constant weight to obtain N-(2-thiopheneethyl)methyleneamine (see its HPLC spectrum in figure 1 ), the yield in this example was 97.1%, and the liquid phase purity was 97.65%.
Embodiment 2
[0050] This embodiment provides a method for synthesizing N-(2-thiopheneethyl)methyleneamine, and the N-(2-thiopheneethyl)methyleneamine is prepared by the following method: adding 100.00 ml of a 250ml three-necked flask to a g 2-thiopheneethylamine, at the same time add 100.00g absolute ethanol (water content 0.34%) and 23.62g paraformaldehyde, under stirring, heat to 49-53 ℃, keep warm for 3h, then suction filtration while hot, the reaction system Naturally cooled to 38°C, white solid was precipitated, then continued to cool to 5-10°C, kept for 2h, suction filtered, and beaten with solvent (0.5 times the mass, temperature 5-10°C) to obtain white solid, which was placed in a blast drying oven (T= 40° C.) and drying to constant weight to obtain N-(2-thiopheneethyl)methyleneamine, the yield in this example is 97.32%, and the liquid phase purity is 99.45%.
Embodiment 3
[0052] This embodiment provides a method for synthesizing N-(2-thiopheneethyl)methyleneamine, and the N-(2-thiopheneethyl)methyleneamine is prepared by the following method: adding 100.00 ml of a 500ml three-necked flask to a g 2-thiopheneethylamine, add 200.00g absolute ethanol (water content 0.34%) and 23.62g paraformaldehyde at the same time, under stirring, heat to 49-53 ℃, keep warm for 3h, then hot suction filtration, the reaction system Naturally cooled to 38°C, white solid was precipitated, then continued to cool to 5-10°C, kept for 2h, suction filtered, and beaten with solvent (0.5 times the mass, temperature 5-10°C) to obtain white solid, which was placed in a blast drying oven (T= 40° C.) and drying to constant weight to obtain N-(2-thiopheneethyl)methyleneamine, the yield in this example is 94.25%, and the liquid phase purity is 99.53%.
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