KR830000244A - Method for preparing sodium salt of oxime derivative of 7-aminothiazolyl acetamido cephalosporanic acid in crystal form - Google Patents

Abstract

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Description

Method for preparing sodium salt of oxime derivative of 7-aminothiazolyl acetamido cephalosporanic acid in crystal form

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Claims (6)

A) Acid of general formula (I) syn isomer, The hydrate, ethanolic salt, phosphate or hydrate of this acid and a mixture of the ethanolic or phosphate NaX (II) (Wherein, X represents an anion of an acid having an acidity comparable to or less than that of acid (I)) of general formula (III) obtained by treatment The hydrated salt of is crystallized, if necessary, in the presence of an excess organic solvent in which the sodium salt is actually insoluble, or; B) An acid of the general formula (I), a hydrate of this acid, an ethanolic or phosphate salt, or a mixture of a hydrate and an ethanolic or phosphate is reacted with sodium of an organic acid in methanol, and the methanolic salt of general formula (III) Isolating the crystalline sodium salt of ), converting this salt to a product of general formula (III) that no longer contains methanol, if necessary, and hydrating the product of general formula (III) or a methanolic salt thereof As the following general formula syn isomer, A hydrated crystalline form, so-called D form, of the compound represented by is prepared, and this form D has a powder X-ray diffraction pattern as follows, and this pattern is obtained by Kα radiation of copper at a wavelength of λ=1.54A°, In this pattern, d has an inner-lattice space, I/I ₁ has a relative intensity, Infrared spectrum as follows in nuzole units Method for producing the D-form having a. A) General formula (I) syn isomer, Of an acid, a hydrate of this acid, an ethanolic salt, or a mixture of a hydrate and an ethanolic salt of the general formula (II) Nax (II) (Wherein X represents an anion of an acid having an acidity comparable to or less than that of acid (I)), and the obtained general formula (III) The hydrated salt of is crystallized by adding an excessive amount of an organic solvent in which the sodium salt is actually insoluble, if necessary, or; B) An acid of the general formula (I), a hydrate of this acid, an ethanolic salt, or a mixture of a hydrate and an ethanolic salt is reacted with the sodium salt of an organic acid in methanol, and the crystalline sodium salt of the general formula (II) is a methanolic salt. And converting this salt to a product of general formula (III) that no longer contains methanol as necessary, and hydrating the product of general formula (III) or a methanolic salt thereof. The method of claim 1 in scope. An acid of formula (I), a hydrate of this acid, an ethanolic salt, or a mixture of a hydrate and an ethanolic salt was treated with sodium of an organic acid in methanol, and the crystalline methanolic salt of the obtained sodium salt was isolated, and the methanolic salt was water A patent claim for manufacturing a harvested crystalline form described in Paragraph 1, characterized in that it is miscible with and is suspended in a solvent containing a small amount of water, and the suspension is left to isolate the desired crystalline form. The method of paragraph 2 of the scope of. The method according to any one of claims 1 to 3, wherein the sodium salt of the organic acid used is selected from the group consisting of sodium acetate, sodium ethyl hexanoate and sodium ethyl acetate. The method of claim 2 or 3, wherein sodium acetate is used as the sodium salt of lactic acid. A method according to claim 3, wherein ethanol containing 1-10% of water is used as a solvent containing a small amount of water in which a methanolic salt is suspended to obtain crystalline form D. A claim characterized in that the treatment of an acid (I), a hydrate of this acid, an ethanolic salt, a phosphate salt, or a mixture of a hydrate and an ethanolic or phosphate salt is performed with a sodium salt at a temperature of about 0°C in an aqueous methanolic solution. The method described in any one of the ranges 1A, 2A, 4 or 5. ※ Note: It is disclosed according to the contents of the initial application.