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4,6-dihydroxypyrimidine synthesizing method

A technology for dihydroxypyrimidine and a synthesis method, which is applied in the field of chemical synthesis, can solve the problems of low yield of the atmospheric pressure method, difficult industrialization of the pressurized method, etc., achieves simple and easy preparation technology, reduces the generation of reaction by-products, improves the The effect of product yield

Inactive Publication Date: 2018-04-03
中山市榄商置业发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing 4,6-dihydroxypyrimidine synthesis methods mainly include normal pressure method and pressurized method. Compared with the malonamide method, the raw materials of these methods are easy to obtain and the yield is relatively high, but the actual yield of the normal pressure method is lower than that of the malonamide method. Low, the industrialization of the pressure method is difficult

Method used

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  • 4,6-dihydroxypyrimidine synthesizing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A kind of synthetic method of 4,6-dihydroxypyrimidine, the concrete steps of this synthetic method are as follows:

[0020] S1: Dissolve 10g of dimethyl malonate in 300ml of sodium methoxide solution, heat up and stir evenly, the temperature of heating up and stirring is 60°C, and the stirring time is 20min;

[0021] S2: Add a catalyst to the solution, turn on the condensed water circulation to lower it to normal temperature, and stir for 15 minutes. The catalyst is a mixture of phosphorus oxychloride, triethylamine and pyrimidine, wherein phosphorus oxychloride: triethylamine: pyrimidine = 3:1 :0.8;

[0022] S3: Use a constant pressure dropping funnel to slowly add 60ml of anhydrous triethylamine dropwise. After the dropwise addition, the temperature rises to react. The dropwise addition of anhydrous triethylamine is completed within 15 minutes, and then the temperature is raised to 60°C;

[0023] S4: After the reaction is over, the solvent is recovered by distillatio...

Embodiment 2

[0027] A kind of synthetic method of 4,6-dihydroxypyrimidine, the concrete steps of this synthetic method are as follows:

[0028] S1: Dissolve 15g of dimethyl malonate in 500ml of sodium methoxide solution, heat up and stir evenly, the temperature of heating up and stirring is 70°C, and the stirring time is 30min;

[0029] S2: Add a catalyst to the solution, turn on the condensed water circulation to lower it to normal temperature, and stir for 20 minutes. The catalyst is a mixture of phosphorus oxychloride, triethylamine and pyrimidine, where phosphorus oxychloride: triethylamine: pyrimidine = 3:1 :0.8;

[0030] S3: Use a constant pressure dropping funnel to slowly add 80ml of anhydrous triethylamine dropwise. After the dropwise addition, the temperature rises to react. The dropwise addition of anhydrous triethylamine is completed within 15 minutes, and then the temperature is raised to 70°C;

[0031] S4: After the reaction is over, the solvent is recovered by distillation ...

Embodiment 3

[0035] A kind of synthetic method of 4,6-dihydroxypyrimidine, the concrete steps of this synthetic method are as follows:

[0036] S1: Dissolve 13g of dimethyl malonate in 400ml of sodium methoxide solution, heat up and stir evenly, the temperature of heating up and stirring is 65°C, and the stirring time is 25min;

[0037] S2: Add a catalyst to the solution, turn on the condensed water circulation to lower it to normal temperature, and stir for 17 minutes. The catalyst is a mixture of phosphorus oxychloride, triethylamine and pyrimidine, where phosphorus oxychloride: triethylamine: pyrimidine = 3:1 :0.8;

[0038] S3: Use a constant pressure dropping funnel to slowly add 70ml of anhydrous triethylamine dropwise. After the dropwise addition, heat up to react. The dropwise addition of anhydrous triethylamine is completed within 15 minutes, and then the temperature is raised to 65°C;

[0039] S4: After the reaction is over, the solvent is recovered by distillation under reduced ...

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Abstract

The invention discloses a 4,6-dihydroxypyrimidine synthesizing method in the technical field of chemical synthesis. The synthesizing method comprises the following specific steps: S1: dissolving 10 to15g of dimethyl malonate into 300 to 500ml of a sodium methylate solution, heating and stirring evenly; S2: adding a catalyst into the solution, opening condensate water circulation to cool to normaltemperature and stirring for 15 to 20min; S3: utilizing constant-pressure dropping funnel to slowly dropwise adding 60 to 80ml of anhydrous triethylamine; S4: performing reduced pressure distillationto recycle a solvent and utilizing sodium hydroxide to adjust a pH value as 6 to7; S5: then performing suction filtration and extracting filtrate by an extracting agent; S6: obtaining 4,6-dihydroxypyrimidine. A preparation technology of the 4,6-dihydroxypyrimidine synthesizing method disclosed by the invention has the advantages of convenience, easiness and practicability; the 4,6-dihydroxypyrimidine synthesizing method has easiness in industrial production; furthermore, reactants can be completely reacted in a reaction process, a product yield can be improved, generation of reaction byproducts is reduced, varieties of mutation factors in the reaction process can be controlled, and quality stability of products is ensured.

Description

technical field [0001] The invention discloses a synthesis method of 4,6-dihydroxypyrimidine, and specifically belongs to the technical field of chemical synthesis. Background technique [0002] 4,6-Dihydroxypyrimidine is a chemical substance, mainly used in fine chemical raw materials and pharmaceutical intermediates. It is used as an intermediate in organic synthesis and used in the pharmaceutical industry to produce sulfamotoxine, a sulfonamide drug. 4,6-dihydroxypyrimidine is also an intermediate of vitamin B4, antineoplastic drugs and auxiliary drugs. The existing 4,6-dihydroxypyrimidine synthesis methods mainly include normal pressure method and pressurized method. Compared with the malonamide method, the raw materials of these methods are easy to obtain and the yield is relatively high, but the actual yield of the normal pressure method is lower than that of the malonamide method. Low, the industrialization of the pressurization method is difficult. For this reason...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/52
CPCC07D239/52
Inventor 梁荣强
Owner 中山市榄商置业发展有限公司