- Preparation method of sarpogrelate hydrochloride intermediate
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The invention discloses a preparation method of sarpogrelate hydrochloride intermediate (2-hydroxy-3'-methoxy diphenylethane). According to the preparation method, m-bromoanisole, ethane, and o-benzyloxybromobenzene are taken as initial raw materials, an inorganic base is taken as an auxiliary agent, a palladium catalyst is adopted for catalysis, and o-benzoxy-3'-methoxy toluylene is obtained via reaction; o-benzoxy-3'-methoxy toluylene is subjected to hydrogenation debenzylation so as to obtain 2-hydroxy-3'-methoxy diphenylethane. The raw materials are common chemical raw materials, are cheap, and are high in safety; separation of by-products obtained in reaction process is relatively simple; separation is complete; steps are few; on-pot-method is adopted; and product yield is increased.
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Paragraph 0039; 0057-0069
(2017/11/29)
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- Method for synthesizing 1-benzyloxy-2-[2-(3-methoxyphenyl) vinyl]benzene
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The invention provides a method for synthesizing 1-benzyloxy-2-[2-(3-methoxyphenyl) vinyl]benzene. The method comprises steps as follows: methyl diphenylphosphinite and m-methoxybenzyl chloride in a mole ratio being 1: (1.1-1.4) are added to a reaction device, are heated to the temperature of 50-70 DEG C under the stirring condition and react for 8-12 h at the temperature of 50-70 DEG C, a product is cooled to the room temperature after reaction, and m-methoxybenzyl diphenylphosphine oxide is obtained; a solvent and an alkalizer are added to m-methoxybenzyl diphenylphosphine oxide, the temperature is controlled in a range of 10-20 DEG C, and the solvent is dropwise added continuously; the materials are subjected to the heat preservation at the temperature of 10-20 DEG C for 6-10 h; the solvent is recovered under the condition of pressure reduction until dryness of the materials, then water is added and stirred, and filtering is performed; the materials are washed to be neutral and dried at the temperature of 55-60 DEG C, and 1-benzyloxy-2-[2-(3-methoxyphenyl) vinyl]benzene is obtained. The synthesizing method is simple and easy to implement, and the reaction is mild.
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Paragraph 0021; 0022
(2016/11/21)
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- Synthesis method of 1-benzyloxy-2-[2-(3-methoxyphenyl)vinyl]benzene
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The invention provides a method for synthesizing 1-benzyloxy-2-[2-(3-methoxyphenyl)vinyl]benzene. The method comprises the following steps: making diphenylmethoxyphosphine react with m-methoxybenzyl chloride at 55-60 DEG C to obtain m-methoxybenzyldiphenylphosphine oxide; adding a solvent and a basifier into the m-methoxybenzyldiphenylphosphine oxide; and keeping reactions at room temperature to obtain 1-benzyloxy-2-[2-(3-methoxyphenyl)vinyl]benzene. The synthesis preparation method is simple, mild in reaction and easy to implement.
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Paragraph 0020;0021
(2016/11/14)
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- Preparation of 1-benzyloxy-2 - [2 - (3-methoxyphenyl) vinyl] phenyltheophylline method (by machine translation)
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The present invention provides a preparation of 1-benzyloxy-2 - [2 - (3-methoxyphenyl) vinyl] phenyltheophylline method, the molar ratio of 1 : 1.1-1.4 diphenyl methoxy phosphorus and between the added to the reaction apparatus for making, to elevate temperature under stirring condition 55-60°C, and at this temperature the reaction 8-12h, after the reaction is cooled to room temperature, between to benzyl diphenyl phosphorusoxychloride; benzyl diphenyl phosphorusoxychloride in the solvent and basifier added, to control the temperature to 10-20°C, continue to dripping solvent; in 10-20 °C lower heat insulating 6-10h; pressure reducing and recovering the solvent to dry, add water to stir and after-filtration; material water to neutral, for 55-60 °C drying to obtain the 1-benzyloxy-2 - [2 - (3-methoxyphenyl) vinyl] benzene. The above-mentioned synthetic preparation method is simple, and the mild reaction, it is easy to realize. (by machine translation)
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Paragraph 0015; 0024; 0025
(2016/11/24)
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- New method for synthesizing 1-benzyloxy-2-[2-(3-methoxyphenyl)vinyl]benzene
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The invention provides a new method for synthesizing 1-benzyloxy-2-[2-(3-methoxyphenyl)vinyl]benzene. The method comprises the following steps: adding diphenylmethoxyphosphine and m-methoxybenzyl chloride in a molar ratio of 1:(1-1.2) into a reaction device; heating to 55-60 DEG C while stirring, and keeping reactions for 10-12h at the temperature; after the reactions, cooling to room temperature to obtain m-methoxybenzyldiphenylphosphine oxide; adding a solvent and a basifier into the m-methoxybenzyldiphenylphosphine oxide, controlling the temperature at 10-20 DEG C and further dropwise adding the solvent; preserving heat for 5-8h at 10-20 DEG C; performing reduced-pressure recovery of the solvent to dryness, and adding water and stirring and filtering; and washing the material to neutrality and drying at 55-60 DEG C to obtain 1-benzyloxy-2-[2-(3-methoxyphenyl)vinyl]benzene. The synthesis preparation method is simple, mild in reactionand easy to implement.
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Paragraph 0024; 0025
(2016/11/24)
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- Synthesis of 1-benzyloxy-2 - [2 - (3-methoxyphenyl) vinyl] phenyltheophylline method (by machine translation)
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The present invention provides a synthetic 1-benzyloxy-2 - [2 - (3-methoxyphenyl) vinyl] phenyltheophylline method, the molar ratio of 1 : 1.05-1.15 diphenyl methoxy phosphorus and between the added to the reaction apparatus for making, to elevate temperature under stirring condition 55-60°C, and at this temperature the reaction 8-12h, after the reaction is cooled to room temperature, between to benzyl diphenyl phosphorusoxychloride; benzyl diphenyl phosphorusoxychloride in the solvent and basifier added, to control the temperature to 10-20°C, continue to dripping solvent; in 10-20 °C lower heat insulating 6-10h; pressure reducing and recovering the solvent to dry, add water to stir and after-filtration; material water to neutral, for 55-60 °C drying to obtain the 1-benzyloxy-2 - [2 - (3-methoxyphenyl) vinyl] benzene. The above-mentioned synthetic preparation method is simple, and the mild reaction, it is easy to realize. (by machine translation)
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Paragraph 0018
(2017/02/24)
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- Synthetic method of sarpogrelate intermediate 2-[2-(3-methoxyphenyl)ethyl]phenol
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The invention discloses a synthetic method of a sarpogrelate intermediate 2-[2-(3-methoxyphenyl)ethyl]phenol and relates to the technical field of organic synthesis. In the method, with m-methoxyl chlorobenzene, which is easy to obtain and is low in cost, as a raw material, the method includes the steps of: 1) performing condensation to the raw material with triethyl phosphite; and 2) performing condensation with o-phenylmethoxyl benzaldehyde (which is prepared from salicylic acid and chlorobenzene), performing hydrogenation to alkylate a double bond, and crystallizing a product with petroleum ether to prepare a white crystal target product. The method simplifies process steps, reduces loss ratio and is 99.5% in product purity. The 2-[2-(3-methoxyphenyl)ethyl]phenol is used for preparing sarpogrelate hydrochloride, wherein single impurity is less than 0.1% in content and the product purity reaches more than 99.8%.
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Paragraph 0008; 0012
(2016/11/02)
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- A practical synthesis of sarpogrelate hydrochloride and in vitro platelet aggregation inhibitory activities of its analogues
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A convenient approach for the preparation of sarpogrelate hydrochloride was developed. Two series of sarpogrelate hydrochloride analogues were designed and synthesized in order to improve their platelet aggregation inhibitory activities, biological tests suggested that these compounds have platelet aggregation inhibitory activities to some extent.
- Chen, Guo Hua,Wang, Sheng,Wu, Fei Hua
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scheme or table
p. 287 - 289
(2010/12/20)
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