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Preparation method of 4,6-dihydroxy-5-methoxypyrimidine sodium

A technology of methoxypyrimidine sodium and dihydroxy, applied in 4 fields, can solve problems such as temperature rise, violent reaction, danger, etc., achieve accurate temperature, increase yield, and suppress side reactions

Inactive Publication Date: 2014-07-09
CHANGSHU NANHU INDAL CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reaction between sodium methoxide, formamide and methyl ethyl methoxymalonate is violent and releases a large amount of heat, which can easily lead to a sharp rise in the temperature in the reactor, resulting in danger, which is not conducive to the safety management of the production workshop

Method used

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  • Preparation method of 4,6-dihydroxy-5-methoxypyrimidine sodium
  • Preparation method of 4,6-dihydroxy-5-methoxypyrimidine sodium

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preparation example Construction

[0025] The preparation method of 4,6-dihydroxy-5-methoxypyrimidine sodium of the present invention comprises the following steps: (a) putting sodium methoxide into a dry container, stirring and heating to 65-68°C, adding formamide , followed by dropwise addition of methyl ethyl malonate, reacting at 65-70°C for 2-6 hours to obtain the mixture; (b) placing the mixture at 25-80°C to distill off methanol, then cooling to 10-15°C, centrifuge to collect the solid. By adding sodium methoxide and formamide in a dry container, and then adding methyl ethyl methoxymalonate dropwise, on the one hand, it can prevent the remaining moisture in the container from destroying the reaction, and on the other hand, the dropwise addition can effectively It is beneficial to control the addition speed of methyl ethyl methoxymalonate, thereby more accurately controlling the temperature of the reaction, suppressing side reactions, and increasing the yield of the desired product.

[0026] In order to ...

Embodiment 1

[0029] This example provides a kind of preparation method of 4,6-dihydroxy-5-methoxypyrimidine sodium, the specific feeding ratio is shown in Table 1:

[0030] Table 1 Reaction raw materials and their feeding ratio

[0031]

[0032] The specific operation process is as follows:

[0033] (a) First put 830kg of sodium methoxide into a dry ring-closure reaction pot, stir and heat to 65-68°C, add 186kg of formamide, and then evenly add methyl ethyl malonate dropwise, and control the dropping temperature to 65°C. ~70°C, dropwise addition time is 1~1.5 hours. After the dropwise addition is completed, keep the reaction at 65-70°C for 4 hours;

[0034] (b) Distill and recover methanol at normal temperature (25-30°C) for 1-1.5 hours, distill at 80°C for 2-3 hours under reduced pressure until methanol does not come out, then add 500L of water, and recover about 0.5-0.5% of methanol with water under normal pressure About 1 hour, when the temperature reaches 80-85°C, stop the distil...

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Abstract

The invention relates to a preparation method of 4,6-dihydroxy-5-methoxypyrimidine sodium. The preparation method comprises following steps: (a) sodium methylate is delivered into a dried container, is stirred and heated to 65 to 68 DEG C, methanamide is added, 2-methoxypropandioic acid ethyl methyl ester is added dropwise, and reaction is carried out at a temperature of 65 to 70 DEG C for 2 to 6h so as to obtain a mixture; and (b) the mixture is subjected to distillation at 25 to 80 DEG C so as to remove methanol, is cooled to 10 to 15 DEG C, and is centrifuged so as to collect a solid material. According to the preparation method of 4,6-dihydroxy-5-methoxypyrimidine sodium, sodium methylate and methanamide are delivered into the dried container, and 2-methoxypropandioic acid ethyl methyl ester is added dropwise, so that on the one hand, damage on reaction caused by residual water in the container is prevented, and on the other hand, the drop-by-drop adding manner is beneficial for controlling of adding speed of 2-methoxypropandioic acid ethyl methyl ester, the reaction temperature can be controlled more accurately, side reaction is inhibited, and yield of needed products is increased.

Description

technical field [0001] The invention relates to a preparation method of a sulfonamide intermediate, in particular to a preparation method of 4,6-dihydroxy-5-methoxypyrimidine sodium. Background technique [0002] Sulfonamide, whose chemical name is 4-(p-aminobenzenesulfonyl)-5,6-dimethoxypyrimidine, is generally used for the treatment of inflammation, such as upper respiratory tract infection tonsillitis, bacillary enteritis, skin infection, etc. It can be used in conjunction with other drugs to treat pulmonary tuberculosis and lymphatic tuberculosis. Sulfonamide has gone through several generations of research and development, and its production process has gradually stabilized, specifically the following preparation steps: [0003] step 1): [0004] [0005] Step (2): [0006] [0007] Step (3): [0008] [0009] Step (4): [0010] [0011] [0012] Step (5): [0013] [0014] Wherein, 4,6-dihydroxy-5-methoxypyrimidine sodium is an intermediate pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/60
CPCC07D239/60
Inventor 邵香民
Owner CHANGSHU NANHU INDAL CHEM
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