562-10-7Relevant articles and documents
Synthesis method of doxylamine succinate
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Paragraph 0056; 0058; 0059; 0061; 0062; 0064-0068, (2019/12/09)
The invention discloses a synthesis method of doxylamine succinate. The method includes: (1) adding 2-pyridylphenylmethylcarbinol into an organic solvent I, adding a catalyst, strong base or alkali metal and 2-dimethylaminochloroethane respectively, performing heating to 100-110DEG C and carrying out reaction for 1-2h; then conducting cooling and filtering; subjecting an aqueous phase to backwashing with the organic solvent I, then performing heating to 70-80DEG C, adding activated carbon for decolorization, then performing filtering, then adding a low-boiling-point organic solvent for extraction, drying the extracted organic phase, and finally conducting reduced pressure concentration at 50-60DEG C to dryness to obtain doxylamine; and (2) dissolving the doxylamine in an organic solvent II, adding succinic acid at 50-60DEG C for reaction, then employing medicinal activated carbon for decolorization and filtering, conducting cooling to a temperature at or below 5DEG C, carrying out stirring crystallization, then performing pumping filtering, and conducting washing with the precooled organic solvent II, and finally performing vacuum drying to obtain the doxylamine succinate. The synthesis method provided by the invention simplifies operation, lowers energy consumption, and has high reaction conversion rate and high yield.
Preparation method of doxylamine succinate
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Paragraph 0048-0050, (2017/01/19)
The invention discloses a preparation method of doxylamine succinate. The preparation method comprises following steps: step 1, 2-pyridyl phenyl methyl carbinol is dissolved in an organic solvent, and is reacted with 2-dimethylaminoethyl chloride hydrochloride at high temperature, after reaction, target product N,N-dimethyl-2-[1-phenyl-1-(2-pyridine)oxethyl]ethylamine is obtained via quenching extracting separation; and step 2, N,N-dimethyl-2-[1-phenyl-1-(2-pyridine) oxethyl]ethylamine obtained in the step 1 and succinic acid are subjected to salt forming in an organic solvent; and finished product N,N-dimethyl-2-(1-phenyl-1-(2-pyridine)ethoxy)ethanamine succinate (doxylamine succinate) is obtained via cooling crystallization. The preparation method is simple, safe, and reliable, is high in doxylamine succinate yield, and is suitable for industrialized enlarged production; and post-treatment is simple and convenient.