- Improved preparation method of nicergoline (by machine translation)
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Compared the prior art,bromonicotinoyl chloride intermediate, is prepared-methoxyphenylglycinol :(1) by a reaction with an organic amine as, an acid-binding agent, to produce 10α -(2) methyl - 101010101010101010and X3B1,methoxyphenylglycinol, in a solvent, 10α - The final yield of the product can reach or above product to be 1 - suitable for large-scale ;(3) production, The, method 5 - comprises the following 5 - steps 5 - carrying out a methylation reaction 1 - with an organic, amine, as an organic amine as an acid,binding compound, in a solvent in a solvent and an inorganic base by an organic amine as an acid-binding agent in, an amide type non-protonic solvent to prepare 50% the . nylmyralyl chloride 99%, midst with an organic amine as an organic amine as an acid-binding agent. (by machine translation)
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Paragraph 0046; 0047; 0050; 0051; 0054; 0055; 0058; 0059
(2020/05/30)
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- Synthetic method of nicergoline
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The invention discloses a synthetic method of nicergoline. The synthetic method comprises the following steps: (1) photocatalytic addition reaction; (2) purification of 10-methoxy-dihydroergosterol; (3) methylation reaction; (4) purification of 10-methoxy-1, 6-dimethane-8-carbinol-ergoline; (5) esterification reaction; and (6) purifying of the nicergoline. According to the Synthetic method of thenicergoline, the mild photocatalytic addition, methylation and esterification reactions in the reaction process are adopted, and the raw materials and reagents with high safety are selected, so that the whole synthesis process is safe and controllable, the post-processing process is simplified, and the product obtained by the reaction is high in yield, high in purity, good in quality and suitablefor industrial production.
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Paragraph 0019-0021
(2020/05/30)
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- New preparation method of 10alpha-methoxy-9,10-MMDL
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The invention discloses a preparation method of 10alpha-methoxy-9,10-MMDL, which is high in product yield, good in product quality, simple in process and suitable for industrial production. The preparation method of 10alpha-methoxy-9,10-MMDL includes the following steps that S1, an intermediate is prepared, wherein lysergic acid and methyl alcohol are subjected to a methoxylation reaction, and after purification, the intermediate 10alpha-methoxy-9,10-dihydrolysergic acid methyl ester is obtained; S2, the intermediate 10alpha-methoxy-9,10-dihydrolysergic acid methyl ester reacts with a reductant, and after purification, 10alpha-methoxy-9,10-MMDL is obtained. By means of the preparation method of 10alpha-methoxy-9,10-MMDL, reaction conditions are mild, operation is easy, the product qualityis good, the product yield is high, the total yield reaches 75% or above, and industrial application and promotion are facilitated.
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Paragraph 0055; 0058; 0059; 0062; 0063; 0068
(2019/03/24)
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- Synthetic method for nicergoline
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The invention discloses a synthetic method for nicergoline. The synthetic method comprises the following steps: allowing lysergol and methanol to generate a methoxylation reaction, and carrying out purifying so as to obtain 10alpha-methoxyl-dihydrolysergol; allowing the 10alpha-methoxyl-dihydrolysergol and trimethylsulphoxonium iodide to generate a methylation reaction, and carrying out purifyingso as to obtain 1-methyl-10alpha-methoxyl-dihydrolysergol; and allowing the 1-methyl-10alpha-methoxyl-dihydrolysergol and 5-bromonicotinoyl chloride to generate an acylation reaction, and carrying outrefining so as to obtain the nicergoline. The synthetic method provided by the invention has the advantages of simple process, mild reaction conditions, easy operation, low toxicity of raw materials,high quality of a finished product, and facilitation of industrial popularization and application.
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Paragraph 0049; 0054
(2018/06/15)
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