- Preparation method of landiolol hydrochloride intermediate
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The invention discloses a preparation method of a high-purity landiolol hydrochloride intermediate N-(2-aminoethyl)-4-morpholinecarboxamide oxalate. The preparation method comprises the following steps: reacting N-phenoxy carbonyl morpholine with ethylenediamine, concentrating the reaction liquid, adding a solvent for dissolving, adjusting the pH value to 9-14 by using alkali, filtering to remove solid byproducts, concentrating the filtrate to obtain N-(2-aminoethyl)-4-morpholine formamide, adding water for dissolving, adjusting the pH value to 1-6 by using oxalic acid, filtering to remove a small amount of ethylenediamine oxalate solid, concentrating the filtrate, adding a solvent, and recrystallizing to obtain the high-purity N-(2-aminoethyl)-4-morpholinecarboxamide oxalate. According to the method, the high-purity landiolol hydrochloride intermediate can be obtained, the defects that the byproduct sodium phenate is difficult to filter, ethylenediamine is easy to remain and the like are overcome, the process is stable and controllable, the solvent can be recycled, and the method is more suitable for industrial production.
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Paragraph 0005; 0021-0025
(2021/06/06)
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- Preparation method of landiolol hydrochloride
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The invention provides a preparation method of landiolol hydrochloride. The preparation method utilizes cheap and easily available raw materials. A key reaction utilizes a phase transfer catalysis method so reaction time is shortened. The preparation meth
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Paragraph 0080; 0092; 0094; 0107; 0109; 0122; 0124
(2017/08/14)
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