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Latamoxef Sodium midbody synthetic method

A technology of latamoxef sodium and a synthetic method, which is applied in the field of preparation of latamoxef sodium, can solve the problems of being unsuitable for industrial production, increasing uncontrollable reaction, and low yield, so as to improve equipment utilization and reduce economic burden , the effect of improving the purity

Inactive Publication Date: 2013-01-16
陕西思尔生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the strong reducing property of tributylphosphine, there is a danger of burning when it encounters high heat, open flame or contact with oxidants; at the same time, due to the addition of a water separation device, the uncontrollability of the reaction increases, and the yield is low and the cost is high.
These disadvantages make the reaction unsuitable for industrial production

Method used

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  • Latamoxef Sodium midbody synthetic method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] see figure 1 , a kind of synthetic method of laoxef sodium intermediate, comprises the following steps:

[0027] 1) Add 150g of toluene, 30g of compound 1 and 12g of triethyl phosphite in sequence to a dry and clean 1L four-necked bottle. After setting up the reflux device, turn on the cooling water and control the internal temperature at 110-120℃, so that the material is refluxed. The reaction is carried out under the state for 4-5h;

[0028] 2) In the above reaction, when the residue of compound 1 is less than or equal to 0.5%, the reaction is completed, then at 50 ~ 55 ℃, reduce the pressure to -0.08MPa and concentrate to evaporate to dryness, then add 300g methanol to the evaporated concentrate, and cool down. To 0 ~ 10 ℃, grow crystals for 1 ~ 2h.

[0029] 3) After the crystal growth is completed, filter, rinse with methanol at 0-5°C, and dry at 50-60°C under negative pressure -0.08MPa for 8-12h to obtain compound 2.

[0030] Using triethyl phosphite as the cata...

Embodiment 2

[0032] A method for synthesizing a laoxef sodium intermediate, comprising the following steps:

[0033] 1) Add 120g of toluene, 30g of compound 1 and 6g of triethyl phosphite in sequence to a dry and clean 1L four-necked bottle. After setting up the reflux device, turn on the cooling water and control the internal temperature at 80-100℃, so that the material is refluxed. The reaction is carried out under the state for 4 to 6 hours;

[0034] 2) When the residue of the above reaction (compound 1) is less than or equal to 0.5%, the reaction is completed, then at 45 ~ 55 ℃, reduce the pressure to -0.08MPa and concentrate to evaporate to dryness, and then add 200g isopropanol to the evaporated concentrate , cooled to 0 ~ 5 ℃, crystal growth for 1.5h.

[0035] 3) After the crystal growth is completed, filter, rinse with isopropanol at 0-5°C, and dry at 50-60°C under negative pressure -0.08MPa for 8-10h to obtain compound 2.

Embodiment 3

[0037] A method for synthesizing a laoxef sodium intermediate, comprising the following steps:

[0038] 1) Add 120g of benzene, 30g of compound 1 and 5g of triethyl phosphite in sequence to a dry and clean 1L four-necked bottle. After setting up the reflux device, turn on the cooling water and control the internal temperature at 80-100℃, so that the material is refluxed. The reaction is carried out under the state for 4 to 6 hours;

[0039] 2) When the residue of compound 1 in the above reaction is less than or equal to 0.5%, the reaction is completed, then at 45 ~ 55 ℃ under reduced pressure -0.08MPa concentrated to evaporate to dryness, then add 200g ethanol to the evaporated concentrate, cool down to 5 ~10℃, grow crystals for 2h.

[0040] 3) After the crystal growth is completed, filter, rinse with ethanol at 0-5°C in a freezer, and dry at 50-60°C under negative pressure -0.08MPa for 8-12 hours to obtain compound 2.

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Abstract

The invention discloses a Latamoxef Sodium midbody synthetic method. The method comprises the following steps: a new desulfurizer-triethyl phosphite is adopted for dehydration reaction in toluene and then is subjected to concentrated crystallization to achieve the purpose of synthesizing [1R-[1a, 5a]]-3-methyl-2-(7-oxo-3-phenyl-4-oxa-2, 6-diazabicyclo [3.2.0] heptane-2-alkene-6-based)-3-butenoic acid methyl ester diphenyl. As the triethyl phosphite is selected as the desulfurizer, the technological process is simplified, the operation is simple and the equipment utilization ratio is high.

Description

technical field [0001] The invention belongs to the technical field of preparation of laoxef sodium, and relates to a method for synthesizing an intermediate of laoxef sodium. Background technique [0002] Laoxacephem sodium is a complete synthetic product, similar in structure to cephalosporins, but S is replaced by O in the parent nucleus. Somewhat similar, stable to beta-lactamase. [0003] The key to the synthesis of laoxefene sodium is to obtain the parent nucleus where S is replaced by oxygen. At present, in the reaction process of preparing the parent nucleus of oxycephem in foreign countries, the main reaction process is 6-APA as raw material, 6-APA→protected amino group →protect the carboxyl group →oxidize the 4-position sulfur atom to obtain the intermediate 6-β-benzamide-4-oxo-penicillic acid diphenylmethyl (compound 1), and then undergo high-temperature ring-opening desulfurization to obtain an important intermediate of the parent nucleus 1R-[1a,5a]]-3-methyl-2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D498/04
Inventor 王作弟
Owner 陕西思尔生物科技有限公司
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