Method for producing pharmaceutical grade dibenzothiazyl disulfide (DM) by using sodium nitrite as oxidant

A technology of sodium nitrite and oxidant, applied in the field of preparing DM, can solve the problems of poor process safety, flammable and explosive toluene, etc., and achieve the effects of high safety, high product purity and simple process

Inactive Publication Date: 2012-02-29
KEMAI CHEM
View PDF8 Cites 7 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004]2. Poor process safety. Toluene is flammable and explosive. Its vapor and air can form an explos

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 100g of rubber accelerator M and 100g of water into the reactor (the weight ratio of the rubber accelerator M is 1:1), add 24g of sodium hydroxide solid (the weight ratio of the accelerator M is 100:24), and the resulting The M sodium salt liquid is filtered through a 200-mesh strainer, and the filtrate is added to the oxidation kettle, and 41.3g of sodium nitrite solid (100:41 with the M weight ratio), 0.03g of catalyzer (the catalyzer is that the mass fraction is 10% ammoniacal liquor dissolving) are added respectively. Catalyst copper acetate, catalyst and M sodium salt weight ratio is 1: 10000), then add 224g water (with M sodium salt liquid weight ratio is 1: 1), under the condition of 20 ℃, stirring speed is 50 rev / min Under the condition, add the sulfuric acid of mass fraction 10% to the oxidation kettle dropwise, the flow rate is controlled at 8m 3 / h, and air was introduced at the same time, and the reaction was controlled within 1 hour. Stop adding the oxi...

Embodiment 2

[0016] Add 100g of rubber accelerator M and 2000g of water into the reactor (the weight ratio of rubber accelerator M is 20:1), add 60g of sodium hydroxide solid (the weight ratio of accelerator M is 100:60), and the resulting The M sodium salt liquid is filtered through a 300-mesh strainer, and the filtrate is added to the oxidation kettle, respectively adding 413g of sodium nitrite (100:410 with the M weight ratio), adding 1.08g of catalyst (the catalyst is a mass fraction of 25% ammonia dissolved catalyst Copper acetate catalyst, with M sodium salt weight ratio is 1: 2000), then add 10080g benzene (with M sodium salt liquid weight ratio is 1: 5), under the condition of 80 ℃, stirring speed is the condition of 1000 rpm Next, add sulfuric acid with a mass fraction of 80% to the oxidation kettle dropwise, and the flow rate is controlled at 1m 3 At the same time, air is introduced into the solution within 20 hours, and the reaction is controlled within 20 hours. Stop adding the...

Embodiment 3

[0018] Add 100g of rubber accelerator M and 1000g of water into the reactor (the weight ratio of the rubber accelerator M is 10:1), add 43.5g of sodium hydroxide (the weight ratio of the rubber accelerator M is 100:43.5), and the resulting M The sodium salt liquid is filtered through a 400-mesh strainer, and the filtrate is added to the oxidation kettle, and 61.9g of sodium nitrite (100:62 with the M weight ratio) and 0.24g of catalyst are added respectively (the catalyst is a catalyst whose mass fraction is 20% ammonia water dissolution). Copper acetate, and M sodium salt weight ratio is 1: 5000), then add 3500g isopropanol (with M sodium salt liquid weight ratio is 1: 3), under the condition of 40 ℃, stirring speed is 150 rev / min Under the condition, add the sulfuric acid of mass fraction 20% to the oxidation kettle dropwise, the flow rate is controlled at 4m 3 Air was introduced at the same time as / h, and the reaction was controlled within 3 hours. Stop adding the oxidant ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a method for producing pharmaceutical grade dibenzothiazyl disulfide (DM) by using sodium nitrite as an oxidant. The method comprises the following steps of: adding water and rubber accelerator M into a reaction kettle in a weight ratio of (1-20): 1, adding sodium hydroxide solid in a weight ratio of the sodium hydroxide solid to the accelerator M of 100: (24-60), reacting, and generating M sodium salt liquid; filtering the solution; adding the filtrate into an oxidation pot, and adding sodium nitrite in a weight ratio of the sodium nitrite to the M of 100: (41-410) and 10 to 25 mass percent copper acetate dissolved by aqueous ammonia, wherein the weight ratio of the catalyst to the M sodium salt is 1: (2,000-10,000); and adding a solvent in a weight ratio of the solvent to the M sodium salt liquid of 1: (1-5), dripping 10 to 80 mass percent of sulfuric acid into the oxidation pot at the temperature of between 20 and 80 DEG C and at the stirring speed of 50 to 1,000 revolutions per minute, controlling the flow rate at 1 to 8m<3>/h, introducing air, controlling the reaction at 1 to 20 hours, and stopping dripping the oxidant solution till the pH value of the solution reaches 4 to 9 hours. According to the method, the solvent is low in loss and has no poison to a person. The purity of the product is over 99 percent, and the melting point of the product reaches over 178 DEG C.

Description

technical field [0001] The invention belongs to a method for preparing DM, in particular to a production technology of pharmaceutical grade DM. Background technique [0002] Pharmaceutical grade DM (dibenzothiazole disulfide) is the production of pharmaceutical intermediates - AE active lipid (2-(2-amino-4-thiazolyl)-2-(methoxyimino) thiobenzothiazolyl acetate) The raw material of the product, AE active lipid product is the raw material for the production of cephalosporin antibiotics. In recent years, the rapid development of cephalosporin antibiotics has stimulated the development of pharmaceutical grade DM. In the patent 200810139264 (a method of preparing pharmaceutical grade DM with industrial grade DM), it is introduced that at present, the production of pharmaceutical grade DM in my country is based on industrial grade DM (dibenzothiazole disulfide) as raw material, with toluene or tetrachloroethylene as the raw material. Solvent, get pharmaceutical grade DM through r...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07D277/78
Inventor 王琰
Owner KEMAI CHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap