Method for preparing sodium, 8-(2-hydroxybenzamido)octanoate

A technology of hydroxybenzamide and sodium caprylate, which is applied in the preparation field of pharmaceutical technology, can solve the problems of low reaction selectivity and yield, high yield of by-products, waste liquid discharge, etc., and achieve improvement of low yield, The effect of high reaction yield and reduced difficulty of separation

Inactive Publication Date: 2015-10-14
CHEMSOON CO LTD
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Problems solved by technology

The main problem of this route is that raw material salicylamide directly reacts with 8-bromooctanoic acid ethyl ester, reaction selectivity and productive rate are very low, by-product productive rate is higher, and separation is very difficult, need to use c

Method used

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  • Method for preparing sodium, 8-(2-hydroxybenzamido)octanoate

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Embodiment Construction

[0017] The present invention will be described in further detail below through examples, and the following examples are explanations of the present invention and the present invention is not limited to the following examples.

[0018] The preparation method of present embodiment 8-(2-hydroxybenzamido) octanoate comprises the following steps:

[0019] step one:

[0020] 30 grams (1 equivalent) of salicylamide was dissolved in 64 milliliters of acetonitrile and 76 milliliters of pyridine, cooled to 0-5 degrees Celsius, slowly added dropwise 26.1 grams (1.1 equivalents) of ethyl chloroformate, slowly warming up to 10 degrees Celsius, and maintained for 30 minutes, Slowly heat up until the internal temperature reaches 90 degrees Celsius, and remove most of the solvent (about 110 milliliters) by water separator distillation until the internal temperature rises to about 124 degrees Celsius, then reduce the temperature to the internal temperature at 90-124 degrees Celsius, keep the r...

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Abstract

The invention discloses a method for preparing sodium, 8-(2-hydroxybenzamido)octanoate which is a drug intermediate. The method comprises the following steps of reacting salicylamide, which serves as a raw material, with ethyl chloroformate to produce an intermediate 2H-benzo[e][1,3]oxazine-2,4(3H)-dione, reacting the intermediate with 8-bromooctanoic acid ethyl ester, carrying out hydrolysis so as to obtain 8-(2-hydroxybenzamido)octanoic acid, and then, reacting 8-(2-hydroxybenzamido)octanoic acid with sodium hydroxide so as to obtain the final product, namely sodium, 8-(2-hydroxybenzamido)octanoate. According to the method, the raw material reacts with ethyl chloroformate to produce the intermediate 2H-benzo[e][1,3]oxazin-2,4(3H)-dione, so that the yield of the reaction is greatly increased, the selectivity of reaction is greatly improved, the production cost is reduced, the production of byproducts is lowered, industrial production is facilitated; and the method is environment-friendly.

Description

technical field [0001] The invention relates to a preparation method in the technical field of medicines, in particular to a preparation method of a medicine intermediate: 8-(2-hydroxybenzamido) octanoic acid sodium. Background technique [0002] 8-(2-Hydroxybenzamido) sodium octanoate, referred to as SNAC, is a dicarbonate compound absorption enhancer, used for the treatment of gastrointestinal diseases, especially suitable for gastrointestinal disorders caused by dicarbonate compound malabsorption. disease. It has been confirmed that oral administration of 8-(2-hydroxybenzamido) octanoate sodium (2.5 mg / day) can effectively treat gastrointestinal diseases caused by malabsorption of dicarbonate phosphate compounds. 8-(2-Hydroxybenzamido) sodium octanoate, as an updated product for the treatment of gastrointestinal dicarbophosphate compound malabsorption, is more effective and safer than the previous drugs, and has a very promising application prospect. [0003] After retr...

Claims

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Application Information

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IPC IPC(8): C07C235/60C07C231/12
Inventor 连锦章辉
Owner CHEMSOON CO LTD
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