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Preparation method of magnesium lithospermate

A technology of pentamagnesium salvianolic acid salt and magnesium ions, which is applied in the field of preparation of pentamagnesium salvianolic acid salt and can solve problems such as chemical synthesis that has not been reported.

Inactive Publication Date: 2013-12-04
SOUTH CHINA AGRI UNIV
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Problems solved by technology

[0014] Data retrieval shows that some scholars have studied the chemical synthesis of salvianolic acid compounds, such as the synthesis of danshensu, salvianolic acid A (Salvianolic acid A) Synthesis of Salvianolic acid B (Salvianolic acid B), Synthesis of Salvianolic acid C (Salvianolic acid C), Synthesis of Salvianolic acid D (Salvianolic acid D), Synthesis of Salvianolic acid F (Salvianolic acid F) etc.; the total chemical synthesis of salvianolic acid E has not been reported

Method used

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  • Preparation method of magnesium lithospermate
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  • Preparation method of magnesium lithospermate

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Embodiment 1

[0068] (1) 3,4-dihydroxybenzaldehyde generates 3,4-dimethoxybenzaldehyde under the action of dimethyl sulfate under heating and reflux, and the reaction equation is as follows

[0069]

[0070] In a 250ml dry three-neck flask, connect the reflux condenser, add 22.63g (0.164mol) of 3,4-dihydroxybenzaldehyde and dissolve it with 200ml of acetone, add 47.47g of potassium carbonate solid, and heat the oil bath to 90℃~ 120°C, with mechanical stirring, and then dropwise added 43.39g (0.344mol) of dimethyl sulfate from a constant pressure dropping funnel. After column separation, 25.1 g of colorless crystals were obtained, with a yield of 92%.

[0071] 1 H-NMR (CDCl 3 400M, ppm): 9.92(s,1H), 7.46(d,1H), 7.42(d,1H), 6.98(d,1H), 3.98(s,3H), 3.92(s,3H).

[0072] (2) 3,4-dimethoxybenzaldehyde reacts with malonic acid to synthesize 3,4-dimethoxyphenylacrylic acid, and the reaction equation is as follows:

[0073]

[0074] Into a 100ml dry three-necked flask, add a stirrer, 3...

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Abstract

The invention discloses a preparation method of pentamagnesium salvianolic acid. The preparation method of the invention comprises the following steps: first synthesizing 3-(3,4-dihydroxy protecting group phenyl)-2-(2,3-dihydroxy Protecting group-6-carboxyvinyl)-2-ethyl acrylate, followed by R-(+)-3-(3,4-dihydroxyprotecting group phenyl)-2-hydroxypropionic acid, S-(-) -3-(3,4-dihydroxy-protecting group phenyl)-2-hydroxypropionic acid undergoes esterification reaction, then removes the hydroxyl protecting group, complexes with magnesium ions, and obtains salvianolic acid pentamagnesium salt. The present invention discloses the chemical total synthesis method of pentamagnesium salvianolic acid salt for the first time, which provides a feasible way for realizing the industrialized production of pentamagnesium salvianolic acid salt; the raw materials of the present invention are easy to obtain, the cost of the synthetic route is relatively low, and the production rate is relatively high .

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to a preparation method of pentamagnesium salvianolic acid. Background technique [0002] Magnesium Salvianolate E mainly exists in Salvia miltiorrhiza. As early as the 1930s, the chemical constituents of Salvia miltiorrhiza were studied abroad. In the late 1970s, domestic scholars extracted, separated and purified the water extract of Salvia miltiorrhiza. Discovered and obtained pentamagnesium salvianolic acid salt, as one of the core active components in the traditional Chinese medicine Salvia miltiorrhiza, it has been confirmed that pentamagnesium salvianolic acid has the following functions: [0003] 1. Protective effect on the heart [0004] Pentamagnesium salvianolic acid can significantly reduce the incidence of arrhythmia after ischemia-reperfusion, reduce the activity of transaminase in the perfusate flowing out of the coronary artery, significantly reduce the destructio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/732C07C67/28
CPCY02P20/55
Inventor 周琢强杨晓云应林张秀琴梁顺全
Owner SOUTH CHINA AGRI UNIV
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