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Preparation method of methotrexate compound

A technology for methotrexate and compounds is applied in the field of preparation of methotrexate compounds, which can solve problems such as low purity of methotrexate, achieve good chlorination catalytic effect, realize rapid separation, and improve catalytic effect.

Active Publication Date: 2021-10-01
ZHEJIANG ZHEBEI PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the problems in the prior art, the present invention provides a preparation method of methotrexate compound, which solves the problem of low purity of methotrexate, utilizes the high-efficiency catalysis of high-activity copper-based catalysts, cooperates with a fixed-bed reaction system, not only The catalytic efficiency is guaranteed, and the rapid separation of the catalyst is realized, which effectively improves the stability of the product

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A preparation method of highly active copper-based catalyst, comprising the steps of:

[0021]b1, in the reaction kettle, add titanium monoxide to 10L of aluminum isopropoxide in toluene and stir to form a suspension evenly, then sweep the water vapor into the reaction kettle until no precipitation occurs, and spray dry to obtain a mixed precipitate Titanium monoxide is a micro-nano powder with a particle size of 10 μm. The concentration of the aluminum isopropoxide in the toluene liquid is 100g / L, and the concentration of the titanium monoxide in the toluene liquid is 100g / L. is 100r / min, the purging speed of the water vapor is 2mL / min, and the temperature is 100°C, the water vapor is passed into toluene to form an aeration system, and the spray amount of the spray drying is 2mL / min, and Stir evenly before spraying, and the drying temperature is 120°C; b2, press the mixed precipitate to form a spherical shape, and then soak it into a sodium hydroxide solution to form a...

Embodiment 2

[0028] A method for preparing a highly active copper-based catalyst, comprising the following steps: b1, in a reaction kettle, adding titanium monoxide to a toluene solution of aluminum isopropoxide and stirring evenly to form a suspension, and then purging water vapor into the reaction vessel In the still, until the precipitation no longer occurs, spray drying to obtain a mixed precipitation; titanium monoxide is a micro-nano powder with a particle diameter of 100nm, and the concentration of the aluminum isopropoxide in the toluene liquid is 200g / L, and the titanium monoxide The concentration of titanium in the toluene liquid is 200g / L, the stirring speed is 200r / min, the purging speed of the water vapor is 4mL / min, and the temperature is 102°C, and the water vapor is passed into the toluene to form an aeration system , the spray amount of the spray drying is 5mL / min, and it is stirred evenly before spraying, and the drying temperature is 130°C; b2, the mixed precipitate is pr...

Embodiment 3

[0035] A preparation method for a highly active copper-based catalyst, comprising the steps of: b1, in a reactor, adding titanium monoxide to 20L of toluene solution of aluminum isopropoxide and stirring to form a suspension evenly, then purging water vapor to In the reaction kettle, until the precipitation no longer occurs, spray drying to obtain mixed precipitation; titanium monoxide is a micro-nano powder with a particle size of 2 μm, and the concentration of the aluminum isopropoxide in the toluene liquid is 150g / L. The concentration of titanium oxide in the toluene liquid is 150g / L, the stirring speed is 150r / min, the purging speed of the water vapor is 3mL / min, and the temperature is 101°C, and the water vapor is passed into the toluene to form aeration system, the spray volume of the spray drying is 4mL / min, and it is stirred evenly before spraying, and the drying temperature is 125°C; b2, the mixed precipitate is pressed to form a spherical shape, and then soaked into t...

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Abstract

The invention belongs to the field of methotrexate synthesis, and particularly relates to a preparation method of a methotrexate compound, which comprises the following steps: under the action of a high-activity copper catalyst, synthesizing p-methylamino benzoyl L-glutamic acid zinc salt from chlorobenzoyl L-glutamic acid, methylamine and zinc chloride, and then synthesizing methotrexate from the p-methylamino benzoyl L-glutamic acid zinc salt, tetraaminopyrimidine sulfate and tribromoacetone, and the preparation method of the chlorobenzoyl L-glutamic acid is limited. According to the method, the problem of low purity of methotrexate is solved, efficient catalysis of the high-activity copper-based catalyst is utilized, and a fixed bed reaction system is matched, so that the catalytic efficiency is ensured, rapid separation of the catalyst is realized, and the stability of the product is effectively improved.

Description

technical field [0001] The invention belongs to the field of synthesis, and in particular relates to a method for preparing methotrexate compounds. Background technique [0002] Methotrexate is an anti-folate antineoplastic drug, which mainly inhibits the synthesis of tumor cells by inhibiting dihydrofolate reductase, thereby inhibiting the growth and reproduction of tumor cells. It has been used to treat childhood leukemia since its discovery in the 1940s, and it has been used in the treatment of psoriasis since the 1950s. It is now a commonly used anti-malignant tumor drug in clinical practice, mainly for acute leukemia, breast cancer, chorionic epithelial Carcinoma and malignant mole, head and neck tumors, bone tumors, leukemic meningospinal infiltration, lung cancer, reproductive system tumors, liver cancer, intractable psoriasis vulgaris, rheumatoid arthritis / autoimmune diseases. [0003] High-purity methotrexate has great significance for its therapeutic effect. Ther...

Claims

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Application Information

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IPC IPC(8): C07D475/08B01J27/122
CPCC07D475/08B01J27/122Y02P20/584
Inventor 王国华谈国军茹凯徐莉锋陈毅军董芳
Owner ZHEJIANG ZHEBEI PHARM CO LTD
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