Preparation method of sulfadoxine

A technology of sulfadoxine and formamide, which is applied in the field of preparation of sulfadoxine, can solve problems such as difficult crystallization and dehydration, equipment corrosion, and human injury, so as to prevent human injury, avoid damage to equipment, and prolong service life Effect

Active Publication Date: 2012-01-11
CHANGSHU JINSHEN MEDICAL PROD CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] According to the analysis of the applicant for many years, one of the reasons for the above-mentioned problem (the related substances are high impurities) is that the product is highly viscous due to the application of the cyclization reaction mother liquor, which makes the impurities wrapped and difficult to separate, and difficult to crystallize and dehydrate. Dry, it is easy to bring impurities into the finished product, and it must be precipitated under acid...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The preparation method of sulfadoxine provided by the invention comprises cyclization reaction and chlorination reaction.

[0027] The ring closure reaction is:

[0028] (1240kg of sodium methoxide solution by weight and mass percent concentration of 32% was put into the reaction pot for the cyclization reaction, and heated to 70°C under stirring, then 310kg of formamide by weight was added, And within 120 minutes (dropping 310 kg of methyl ethyl malonate by weight, the reaction temperature (also called dropping temperature) when adding methyl ethyl malonate dropwise is controlled at 75°C , heat preservation, that is, heat preservation reaction for 6 hours, then recover methanol until all water is added, continue to recover methanol until no fraction drips out, cool and crystallize, the temperature of cooling and crystallization is

[0029] The chlorination reaction is:

[0030] Put 857.5kg of phosphorus oxychloride by weight into a dry reactor and heat it ...

Embodiment 2

[0032] The preparation method of sulfadoxine provided by the invention comprises cyclization reaction and chlorination reaction.

[0033] The ring closure reaction is:

[0034] 1085kg of sodium methoxide solution by weight and with a mass percentage concentration of 29.5% was put into the reaction pot for the cyclization reaction, and heated to 65°C under stirring, and then 232.5kg of formamide by weight was added, And within 90 minutes, 294.5kg of methyl ethyl malonate by weight is added dropwise, and the reaction temperature (also called the dropping temperature) when adding methyl ethyl malonate dropwise is controlled at 70°C , heat preservation, that is, heat preservation reaction for 5 hours, then recover methanol until all water is added, continue to recover methanol until no fraction drips out, cool and crystallize, the cooling crystallization temperature is

[0035] The chlorination reaction is:

[0036] Put 796kg of phosphorus oxychloride by weight into a...

Embodiment 3

[0038] The preparation method of sulfadoxine provided by the invention comprises cyclization reaction and chlorination reaction.

[0039] The ring closure reaction is:

[0040] 930kg of sodium methoxide solution by weight and with a mass percentage concentration of 27% was put into the reaction pot for the ring closure reaction, and heated to 60°C under stirring, then 155kg of formamide by weight was added, and Add 279 kg of methyl ethyl malonate by weight dropwise within 60 minutes, and the reaction temperature (also called the dropping temperature) when adding methyl ethyl malonate dropwise is controlled at 65°C and kept warm That is, heat preservation reaction for 4 hours, then recover methanol until all water is added, continue to recover methanol until no fraction drips out, cool and crystallize, the temperature of cooling and crystallization is

[0041] The chlorination reaction is:

[0042] Put 735kg of phosphorus oxychloride by weight into a dry reactor and...

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PUM

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Abstract

A preparation method of sulfadoxine belongs to the field of sulfanilamide antimicrobial drug preparation. Cyclization reaction comprises the following steps of: firstly pouring a sodium methoxide solution into a reactive pan, then successively adding methanamide and methyl ethyl methoxymalonate, keeping warm, recovering methanol, cooling for crystallization, drying by centrifugation, discharging,and drying to obtain 5-methoxy-4,6-disodium dihydroxypyrimidine; Chlorination reaction comprises the following steps of: firstly putting phosphorus oxychloride into a reaction vessel for heating, adding 5-methoxy-4,6-disodium dihydroxypyrimidine into the reaction vessel to react, decompressing and recovering phosphorus oxychloride until the material is dry, cooling, adding trichloro ethylene withuniformly stirring, putting into a hydrolysis pan for hydrolyzation, collecting a trichloro ethylene layer after standing and delaminating, followed by a neutralization reaction, controlling pH value, washing, removing a water layer, recovering trichloro ethylene, and releasing crystals to obtain 5-methoxy-4,6-dichloropyrimidine. The preparation method provided by the invention can be used to guarantee the product purity, prolong the service life of equipment, avoid the damage to the environment and human body, reduce emission, and save energy, and accords with foreign pharmacopoeia standard requirements.

Description

technical field [0001] The invention belongs to the technical field of preparation of sulfonamide antibacterial drugs, and in particular relates to a preparation method of sulfadoxine. Background technique [0002] The chemical name of sulfadoxine (SDM) is: 4-(p-aminosulfonamide) 5,6-dimethoxypyrimidine; the English name is: Sulfadoxine; the Latin name is: Sulphamethoxinum or Sulfadimoxine; the molecular formula is C 12 h 14 o 4 N 4 S; molecular weight 310.33. [0003] Sulfadoxine, also known as Zhouxiao sulfonamide, sulfa-o-dimethoxine or 4-sulfa-5,6-dimethoxypyrimidine, is a white or off-white crystalline powder with a slightly bitter taste, odorless, and gradually changes color when exposed to light. Slightly soluble in water, methanol and ethanol, insoluble in ether, soluble in sodium hydroxide and dilute inorganic acids, belonging to sulfonamide antibacterial drugs. Sulfadoxine has the characteristics of long curative effect and low toxicity. It can tre...

Claims

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Application Information

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IPC IPC(8): C07D239/34C07D239/69
Inventor 李涛
Owner CHANGSHU JINSHEN MEDICAL PROD CO LTD
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