A kind of preparation method of sulfasalazine intermediate

A technology for sulfasalazine and intermediates, applied in the field of preparation of sulfasalazine intermediates, can solve the problems of increased production cost, complicated production process, long production time and the like, and has the advantages of short reaching time, low process temperature and low manufacturing cost. low effect

Active Publication Date: 2022-03-11
SUZHOU HUANGHE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The current method for producing sulfasalazine needs to be mixed and manufactured through various intermediates, and some catalysts or solvents with chronic toxicity need to be added, which is not friendly to the environment and increases production costs; in addition, the production process is more cumbersome and the production time is longer. long, not conducive to industrialization

Method used

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Examples

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Effect test

preparation example Construction

[0022] The invention provides a kind of preparation method of sulfasalazine intermediate, comprising the following steps:

[0023] Step 1: Add 4-amino-7-chloroquinoline into a mixing container filled with an organic solvent, pass an inert gas into the mixing container, and raise the temperature to 65-75°C;

[0024] Step 2: After stirring for a certain period of time, add side chains and catalysts to the mixing container, continue to heat up to 85±3°C, and continue stirring;

[0025] Step 3: After the reaction is finished, cool down to 10±2°C and stand for separation to obtain the hydroxychloroquine matrix;

[0026] Step 4: adding sulfate solution to the hydroxychloroquine matrix, stirring for 3.5-5 hours, and separating the solids in the solution, further drying to obtain hydroxychloroquine sulfate material.

[0027] The hydroxychloroquine sulfate can be used as a sulfasalazine intermediate, which can replace chronic toxic catalysts or solvents.

[0028] In the present inven...

Embodiment 1

[0034] Add 10g of 4-amino-7-chloroquinoline into a mixing container containing 150g of dichloromethane, feed nitrogen into the mixing container, and heat up to 65°C; after stirring for a certain amount of 50min, add 5- (N-ethyl-N-hydroxyethyl)-2-aminopentane and catalyst DMPA, continue to heat up to 85°C, continue to stir for 20min; cool down to 70°C and react for 2.5h, further cool down to 10±2°C and stand still Place and separate the aqueous phase and the organic phase in the mixture to obtain the hydroxychloroquine base; add copper sulfuric acid to the hydroxychloroquine base, stir for 2.5h, and separate the solids in the mixed solution, and further dry to obtain the hydroxychloroquine sulfate material; The yield of chloroquine sulfate material is 89%, HPLC≥92%.

Embodiment 2

[0036] Add 20g of 4-amino-7-chloroquinoline into a mixing container containing 300g of trichloroethane, pass nitrogen gas into the mixing container, and raise the temperature to 70-75°C; after stirring for 55min, add 5-(N-ethyl-N-hydroxyethyl)-2-aminopentane and catalyst DMA, continue to heat up to 87°C, continue to stir for 15min; cool down to 65°C and react for 3h, further cool down to 10±2°C and Stand to separate the aqueous phase and the organic phase in the mixture to obtain the hydroxychloroquine matrix; add ferrous sulfuric acid to the hydroxychloroquine matrix, stir for 2.5 hours, and separate the solids in the mixed solution, and further dry to obtain the hydroxychloroquine sulfate material ; The yield of hydroxychloroquine sulfate material is 94%, HPLC≥95%.

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PUM

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Abstract

The present invention provides a kind of preparation method of sulfasalazine intermediate, and its preparation method comprises the following steps: Step 1: add 4-amino-7-chloroquinoline in the mixing container that organic solvent is housed, add to described mixing container Inert gas is introduced into the medium, and the temperature is raised to 65-75°C; Step 2: After stirring for a certain period of time, add side chains and catalysts to the mixing container, continue to heat up to 85±3°C, and continue to stir; Step 3: Wait for the reaction After the end, cool down to 10±2°C and stand for separation to obtain the hydroxychloroquine matrix; Step 4: add sulfate solution to the hydroxychloroquine matrix, stir for 3.5-5 hours, and separate the solids in the solution, and further bake Dry access to hydroxychloroquine sulfate material. The preparation method of the sulfasalazine intermediate of the present invention has a simple preparation process and is suitable for popularization and use.

Description

technical field [0001] The invention provides a preparation method of a sulfasalazine intermediate, which belongs to the technical field of chemical industry. Background technique [0002] Sulfasalazine (SASP), also known as 5-[p-(2-pyridinesulfamoyl)benzene]azosalicylic acid. Molecular formula is C18H14N4O5S, molecular weight: 398.39. [0003] Sulfasalazine is an azo compound of salicylic acid and sulfapyridine, which has antibacterial, antirheumatic and immunosuppressive effects. In the intestinal tract, it is decomposed by the bacteria there into sulfapyridine (SP) and 5-aminosalicylic acid (5-ASA). [0004] The current method for producing sulfasalazine needs to be mixed and manufactured through various intermediates, and some catalysts or solvents with chronic toxicity need to be added, which is not friendly to the environment and increases production costs; in addition, the production process is more cumbersome and the production time is longer. Long, not conducive ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D215/46
CPCC07D215/46
Inventor 肖祖华江尔胜
Owner SUZHOU HUANGHE PHARMA CO LTD
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