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Preparation method of menadione dimethylpyrimidinol bisulfite

A technology of dimethylpyrimidinol menadione sulfite and menadione sodium bisulfite, which is applied in the field of vitamin K3 processing and preparation, and can solve the problems of easy moisture absorption, lack of systematic and reasonable preparation methods, poor stability, etc.

Inactive Publication Date: 2018-09-21
SHANDONG HUASHENG CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

MSB has poor stability and is easy to absorb moisture
MNB and MPB have better stability. At the same time, there are many reports about the synthesis of MNB, but there are few reports about the preparation method of MPB, and there is a lack of systematic and reasonable preparation methods.

Method used

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  • Preparation method of menadione dimethylpyrimidinol bisulfite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1, the present embodiment provides a kind of preparation method of dimethylpyrimidine alcohol menadione sulfite

[0016] First, weigh the required water, menadione sodium bisulfite, 4,6-dimethyl-2-hydroxypyrimidine hydrochloride, 4,6-dimethyl-2-hydroxypyrimidine hydrochloride according to the proportion The consumption is consistent with the molar weight of sodium bisulfite menaquinone, and the consumption of water is 5 times of the weight of sodium bisulfite menaquinone, and in the above-mentioned raw materials, sodium bisulfite menaquinone is a kind of vitamin K3, 4, 6-Dimethyl-2-hydroxypyrimidine hydrochloride is a material intermediate, mainly used for the production of nicarbazine. Nicarbazine is a highly efficient, low toxicity, does not affect immune function, and slow production of drug-resistant insect beads. Anticoccidial drug, 4,6-dimethyl-2-hydroxypyrimidine hydrochloride is one of the intermediates in the preparation of nicarbazine.

[0017] The...

Embodiment 2

[0021] Embodiment 2, the present embodiment provides a kind of preparation method of dimethylpyrimidine alcohol menadione sulfite

[0022] First, weigh the required water, menadione sodium bisulfite, 4,6-dimethyl-2-hydroxypyrimidine hydrochloride, 4,6-dimethyl-2-hydroxypyrimidine hydrochloride according to the proportion The consumption is 1.1 times the molar weight of sodium bisulfite menaquinone, and the consumption of water is 6 times the weight of sodium bisulfite menadione.

[0023] Then, the above-mentioned weighed raw materials were added to the reaction kettle, and the temperature was controlled at 20° C. and the time was between 2 hours to obtain a solution of menadione dimethyl pyrimidinol sulfite;

[0024] Then, the dimethylpyrimidinol menadione sulfite solution obtained by the reaction is cooled to 20°C and warmed to about 15°C (fluctuation up and down ±1°C), and vacuum filtration is adopted to obtain a filter cake;

[0025] Finally, the filter cake was washed wit...

Embodiment 3

[0026] Embodiment 3, the present embodiment provides a kind of preparation method of dimethylpyrimidine alcohol menadione sulfite

[0027] First, weigh the required water, menadione sodium bisulfite, 4,6-dimethyl-2-hydroxypyrimidine hydrochloride, 4,6-dimethyl-2-hydroxypyrimidine hydrochloride according to the proportion The consumption is 1.2 times the molar weight of sodium bisulfite menaquinone, and the consumption of water is 7 times the weight of sodium bisulfite menadione.

[0028] Then, the above-mentioned weighed raw materials were added to the reaction kettle, and the temperature was controlled at 50 ° C and the time was between 2 h to obtain a solution of menadione dimethyl pyrimidol sulfite;

[0029] Then, the dimethylpyrimidinol menadione sulfite solution obtained by the reaction is cooled to 10°C and warmed to about 15°C (up and down fluctuation ±1°C), and vacuum filtration is adopted to obtain a filter cake;

[0030] Finally, the filter cake was washed with wate...

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Abstract

The invention belongs to the field of processing and preparation of vitamin K3, and in particular relates to a preparation method of menadione dimethylpyrimidinol bisulfite. The preparation method comprises the following valid steps: a. adding water, menadione sodium bisulfite and 2-hydroxy-4,6-dimethylpyrimidine hydrochloride into a reaction kettle, controlling the temperature to be 20-40 DEG C,and controlling the time to be 1-2h; b. then, cooling to 10-20 DEG C, and filtering to obtain a filter cake; c. washing the filter cake and then drying under the temperature of 5 to 10 DEG C to obtainthe white or almost white menadione dimethylpyrimidinol bisulfite finished product. The preparation utilizes the widely used menadione sodium bisulfite as the raw material, and enables the menadionesodium bisulfite to react with the 2-hydroxy-4,6-dimethylpyrimidine hydrochloride, so that the menadione dimethylpyrimidinol bisulfite is prepared, and the technical problem of lack of a MPB system and reasonable preparation methods can be solved; furthermore, the preparation method provided by the invention is simple, reliable and suitable for large-scale popularization and use.

Description

technical field [0001] The invention belongs to the field of vitamin K3 processing and preparation, and in particular relates to a preparation method of menadione dimethylpyrimidinol sulfite. Background technique [0002] Vitamin K3 is the collective name for 2-methyl-1,4 naphthoquin (referred to as menadione) and its adducts. The function of vitamin K3 is to promote blood coagulation, and the level of prothrombin in the blood is directly related to the supply of vitamin K3. Animals deficient in vitamin K3 have significantly prolonged clotting time, and in severe deficiencies, minor abrasions can cause continuous bleeding and lead to death. Hormones and antibiotics are often added to the existing feed, which results in the lack of vitamin K3 in animals. Therefore, it is necessary to add vitamin K3 to the feed to supplement the content of vitamin K3 in animals. [0003] At present, vitamin K3 as feed additive includes sodium bisulfite menadione (MSB), nicotinamide bisulfite...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/36C07C50/12C07C46/00C07C309/25C07C309/44C07C303/32A23K20/174
CPCA23K20/174C07C46/00C07C50/12C07C303/32C07C309/25C07C309/44C07C2602/10C07D239/36
Inventor 谢瑞兴孙新科张自恒
Owner SHANDONG HUASHENG CHEM TECH