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Synthesis method of methoxamine hydrochloride

A technology of methoxamine hydrochloride and synthesis method, which is applied in the field of organic chemical synthesis, can solve the problems of restricting wide application, etc., and achieve the effects of high yield, easy scale-up production, and stable scale-up production

Active Publication Date: 2009-04-29
NANCHANG HANGKONG UNIVERSITY
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Problems solved by technology

The innovations of the two have jointly promoted the development of the social economy. The former has reported that dimethyl sulfate and potassium iodide have been used as methylation reagents to achieve good results, but they are highly toxic chemical reagents and require special procedures. procedures and formalities can only be applied, which greatly limits their widespread application

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  • Synthesis method of methoxamine hydrochloride

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Embodiment Construction

[0014] 1. Preparation of p-dimethoxybenzene: under nitrogen protection, add 33.6 grams of potassium carbonate and 90 grams of industrial acetonitrile in a 0.5-liter clean and water-free four-necked bottle, stir for 5 minutes, and then add 44.5 grams of liquid For methyl p-toluenesulfonate, wash the mouth of the bottle with 10 g of acetonitrile. Stir for 5 minutes, control the temperature to 15°C±3°C, and add 104.7g of acetonitrile mixture containing 16.7g of hydroquinone dropwise (about 1 hour). Stirring for another 5 minutes, the temperature was raised to 83° C. and the reaction was vigorously refluxed, and the nitrogen gas was turned off when reflux occurred. At this time, when gas is generated, the system becomes a pale yellow-white turbid liquid. TLC plate (ethyl acetate: dichloromethane = 1:30), until the raw material point (mung bean point) disappears, that is, the reaction is complete. After about 22 hours, the reaction was completed, and then the temperature was lowe...

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Abstract

The invention discloses a novel synthesis method for methoxamine hydrochloride, which comprises the following steps: under the protection of nitrogen, liquid methyl p-toluenesulfonate is added into certain amount of acetonitrile solution of potassium carbonate, the temperature is controlled to between 12 and 18 DEG C, and proper amount of acetonitrile mixed liquid of hydroquinone is slowly dripped. Then the stirring is performed for 5 minutes, the temperature is increased to 83 DEG C for violent reflux reaction, the nitrogen is turned off when the reflux appears, and the complete reaction can be finished 22 hours later. Then a Friedel-Crafts acylation reaction, an oximation reaction, a hydroximino reduction reaction and a ketoamine hydrogenation reaction are orderly performed, and finally a target product is synthesized by an economical and environment-friendly route. The yields of 5-step operations are 94 percent, 72 percent, 80 percent, 79 percent and 88 percent respectively. The method has the advantages that the method has mild reactions and simple conditions, is steady and easy for scale-up production, and improves the yield compared with the prior synthesis of the methoxamine hydrochloride.

Description

technical field [0001] The invention relates to an organic chemical synthesis method, in particular to a synthesis method of methoxamine hydrochloride. Background technique [0002] Methoxamine hydrochloride is a commonly used drug for regulating vasoconstriction and improving blood pressure. There is no report on its total synthesis in domestic literature, and foreign countries mostly use some classic reactions to study its conditions to obtain a relatively ideal yield. For example, using Dimethyl sulfate for methylation. Although it has taken a firm step forward technically, it has not taken into account its practical reality. The invention starts from the most readily available raw materials, synthesizes the target product through multi-step reactions and research on reaction conditions, and improves the reaction yield compared with the synthesis of traditional methoxamine hydrochloride. The most prominent place is the selection of methyl p-toluenesulfonate, which has n...

Claims

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Application Information

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IPC IPC(8): C07C217/70C07C213/00
Inventor 谢宇胡金刚李明俊魏娅
Owner NANCHANG HANGKONG UNIVERSITY
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