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It is a common heterocyclic compound, the isothiazole compound, Sodium 3-oxido-5-sulfidoisothiazole-4-carboxylate, cas is 76857-14-2 its synthesis route is as follows.

4-carboxy-5-mercapto-3-hydroxy-isothiazolium trisodium (5) (24.31 g, 0.10 mol) was added to a solution of(About 65ml) hydrochloric acid stirring, the pH to 2-3, by adding 297mgDMAPStirring was continued for 20 minutes,Followed by addition of 50 ml of tert-butanol,6 ml of pyridine, Boc2O (21.83 g, 0.10 mol),In a dry environmentThe reaction was stirred at room temperature for 18 h. The reaction was complete by HPLC and the solvent was removed by rotary evaporation to give an oil which was chromatographed on ethyl acetate, The organic layer was dried over anhydrous magnesium sulfate, concentrated, and recrystallized from ethanol to give Intermediate 6 (24.11 g) in a molar yield87%, HPLC purity 99.2%.

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Reference£º
Patent; Shandong Luoxin Pharmaceutical Group Co Ltd; Sun, Song; Xu, Qinyan; Chang, Zhicheng; (7 pag.)CN105646544; (2016); A;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

 

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A head spore for the Tanzania acid new crystalline and its preparation method (by machine translation)

A head spore for the Tanzania acid new crystalline and its preparation method. The present invention provides a [6R – (6a, 7 alpha)] – 7 – [[ [4 – (2 – amino – 1 – carboxyl – 2 – oxo ethylidene) – 1, 3 – dithio-azetidine – 2 – yl] carbonyl] amino] – 7 – methoxy – 3 – [[ (1 – methyl – 1H – tetrazol – 5 – yl) thio] methyl] – 8 – oxo – 5 – thia – 1 – azabicyclo [4, 2, 0] Oct – 2 – ene – 2 – carboxylic acid the new crystalline form, this crystalline form X – ray powder diffraction pattern of a reflection angle of the 2 theta in the 11.66 ¡À 0.1 , 17 . 53 ¡À 0.1 , 17 . 72 ¡À 0.1 , 18 . 91 ¡À 0.1 , 20 . 01 ¡À 0.1 , 21 . 02 ¡À 0.1 , 22 . 24 ¡À 0.1 , 23 . 33 ¡À 0.1 and has a characteristic peak. Such a compound is crystalline form has good stability, and its preparation process is simple, lower cost, can be used in industrial production. (by machine translation)

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Reference£º
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com

 

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A amorphous head spore for the Tanzania acid and prepared cefotetan disodium method and containing the cefotetan disodium pharmaceutical composition (by machine translation)

The invention discloses a head-spore for the Tanzania acid new crystal and prepared cefotetan disodium method and containing cefotetan disodium pharmaceutical composition. The new crystalline form X – ray diffraction pattern in the X – ray diffraction does not occur, and in the differential thermal analysis endothermic peak for the Atlas 158.3 C, exothermic peak at 144.6 C. The new crystalline form of the present invention solved in the prior art by the header spore for the Tanzania acid prepared cefotetan disodium is unstable. The invention the preparation method used good operability, organic less solvent residue, is very suitable for large-scale industrial production. (by machine translation)

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Reference£º
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com

 

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Cefotetan disodium preparation method (by machine translation)

The invention discloses a cefotetan disodium preparation method, comprises the following steps: (1) preparing 1st intermediate; (2) the extraction separation; (3) preparing 2nd intermediate; (4) crystallization separation; (5) the crude preparation head spore for the tanzania acid; (6) head spore for the tanzania acid purification; (7) preparation head spore for the tanzania acid disodium. The invention relates to a cefotetan disodium preparation method, the process is simple, mild reaction conditions, the reaction process of the good controllability, the product yield is high, the resulting cefotetan disodium high purity, low impurity content, good appearance quality, stable property, clinical it has broad application prospects. (by machine translation)

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Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com

 

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A and Cefotetan disodium method for the preparation of intermediates (by machine translation)

The invention discloses a Cefotetan disodium method for the preparation of intermediates thereof, the commercial raw material 4 – (1-amino-3-tert-butoxy -1,3-dioxo-2-ene yl) – 1,3-dithio-azetidine-2-carboxylic acid (2) and 7-MAC (3) for a condensation reaction to make compound 4, after deprotection, salification Cefotetan disodium (1). The invention also provides the compound 2 preparation method. The conventional route of the route to avoid pollution of the environment of the use of chloride reagent, with simple process route, process cost reduction, the overall yield of product is improved, friendly characteristic of the environment, is suitable for industrial production. (by machine translation)

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Reference£º
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com

 

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Process for obtaining compounds usable in the production of cefotetan, and new compounds obtained thereby

A process for obtaining salts of 4-carboxy-3-hydroxy-5-mercapto-isothiazole which are compounds usable in the production of Cefotetan, and new compounds obtained thereby, in which R1 = R2 = R3 = Na or K; R1 = Na or K and R2 = R3 = H; or R1 = R2 = Na or K and R3 = H.

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Reference£º
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com

 

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Cefotetan disodium preparation method (by machine translation)

The invention discloses a cefotetan disodium preparation method, comprises the following steps: (1) preparing 1st intermediate; (2) the extraction separation; (3) preparing 2nd intermediate; (4) crystallization separation; (5) the crude preparation head spore for the tanzania acid; (6) head spore for the tanzania acid purification; (7) preparation head spore for the tanzania acid disodium. The invention relates to a cefotetan disodium preparation method, the process is simple, mild reaction conditions, the reaction process of the good controllability, the product yield is high, the resulting cefotetan disodium high purity, low impurity content, good appearance quality, stable property, clinical it has broad application prospects. (by machine translation)

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Reference£º
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com

 

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A amorphous head spore for the Tanzania acid and prepared cefotetan disodium method and containing the cefotetan disodium pharmaceutical composition (by machine translation)

The invention discloses a head-spore for the Tanzania acid new crystal and prepared cefotetan disodium method and containing cefotetan disodium pharmaceutical composition. The new crystalline form X – ray diffraction pattern in the X – ray diffraction does not occur, and in the differential thermal analysis endothermic peak for the Atlas 158.3 C, exothermic peak at 144.6 C. The new crystalline form of the present invention solved in the prior art by the header spore for the Tanzania acid prepared cefotetan disodium is unstable. The invention the preparation method used good operability, organic less solvent residue, is very suitable for large-scale industrial production. (by machine translation)

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Reference£º
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com

 

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A head spore for the Tanzania acid new crystalline and its preparation method (by machine translation)

A head spore for the Tanzania acid new crystalline and its preparation method. The present invention provides a [6R – (6a, 7 alpha)] – 7 – [[ [4 – (2 – amino – 1 – carboxyl – 2 – oxo ethylidene) – 1, 3 – dithio-azetidine – 2 – yl] carbonyl] amino] – 7 – methoxy – 3 – [[ (1 – methyl – 1H – tetrazol – 5 – yl) thio] methyl] – 8 – oxo – 5 – thia – 1 – azabicyclo [4, 2, 0] Oct – 2 – ene – 2 – carboxylic acid the new crystalline form, this crystalline form X – ray powder diffraction pattern of a reflection angle of the 2 theta in the 11.66 ¡À 0.1 , 17 . 53 ¡À 0.1 , 17 . 72 ¡À 0.1 , 18 . 91 ¡À 0.1 , 20 . 01 ¡À 0.1 , 21 . 02 ¡À 0.1 , 22 . 24 ¡À 0.1 , 23 . 33 ¡À 0.1 and has a characteristic peak. Such a compound is crystalline form has good stability, and its preparation process is simple, lower cost, can be used in industrial production. (by machine translation)

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Reference£º
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com

 

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Process for obtaining compounds usable in the production of cefotetan, and new compounds obtained thereby

A process for obtaining salts of 4-carboxy-3-hydroxy-5-mercapto-isothiazole which are compounds usable in the production of Cefotetan, and new compounds obtained thereby, in which R1 = R2 = R3 = Na or K; R1 = Na or K and R2 = R3 = H; or R1 = R2 = Na or K and R3 = H.

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Reference£º
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com