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Preparation of Leiliqusai

A preparation process and technology of raltitrexed, applied in the field of medicine, can solve the problems of low yield, harsh reaction conditions, affecting the popularization and application of raltitrexed, etc., and achieves reduction of production cost, mild reaction conditions, and improved synthesis yield. rate and quality of finished products

Inactive Publication Date: 2004-12-08
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The current raw material synthesis process of raltitrexed has shortcomings such as low yield and harsh reaction conditions, which affect the promotion and application of raltitrexed

Method used

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  • Preparation of Leiliqusai
  • Preparation of Leiliqusai
  • Preparation of Leiliqusai

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0017] Preparation of intermediate 2 (methyl 5-nitro-thiophene-2-carboxylate): under ice-salt cooling, 173g Add to 1000ml of methanol, drop 75ml of SOCl at less than -10°C 2 After the addition, the reaction was carried out overnight at room temperature, the solvent was evaporated to dryness, and the intermediate 2 was obtained by distillation under reduced pressure with a yield of 91.7%. The reaction formula is as (1):

[0018]

example 2

[0020] Preparation of intermediate 3 (methyl 5-aminothiophene-2-carboxylate): dissolve the product obtained in Example 1 (intermediate 2) in 200 ml of methanol, add 1 g of 10% palladium carbon, catalytic hydrogenation, filter, and evaporate to dryness Solvent was used to obtain intermediate 3 with a yield of 89.3%. The reaction formula is as (2):

[0021]

example 3

[0023] Preparation of intermediate 4 (5-(N-acetyl-)-aminothiophene-2-carboxylic acid methyl ester): the product obtained in the above example 2 (intermediate 3) was dissolved in HOAc, and an equivalent amount of acetic anhydride was added dropwise, Stir at room temperature until the reaction of the raw materials is complete, and evaporate the solvent to obtain intermediate 4 with a yield of 87.9%. The reaction formula is as (3):

[0024]

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Abstract

A process for preparing Leitiqusai from 5-nitro-thiophene-2-formate through esterifying, nitro reduction, acetylation, methylation, hydrolysis, esterification nucleophilic substitution, hydrolysis, acylation, amide nucleophilic substitution, hydrolysis and acidification. Its advantages are high output rate and low cost.

Description

technical field [0001] The invention provides a new preparation process of raltitrexed, which belongs to the technical field of medicine. Background technique [0002] Colorectal cancer is one of the common malignant tumors and is a common cancer in Western countries. With the development of my country's economy and the change of people's lifestyle and dietary structure, the incidence rate is increasing year by year, especially in recent years, with a rate of 4%. In 1993, according to the results of the malignant tumor death survey in my country, the mortality rate of colorectal cancer in both urban and rural areas was higher than that of the 1973 death retrospective survey. Epidemiological studies have found that countries with a high incidence of colorectal cancer have a diet high in fat and low in cellulose, other environmental factors (such as molybdenum deficiency in soil), schistosomiasis, colorectal adenoma, pelvic radiation, inflammation, smoking, etc. It is also r...

Claims

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Application Information

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IPC IPC(8): C07D409/12
Inventor 赵志全
Owner LUNAN PHARMA GROUP CORPORATION
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