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Novel method for preparing ethambutol hydrochloride

A technology for ethambutol hydrochloride and ethambutol, which is applied in the field of preparing ethambutol hydrochloride, and can solve the problems of multiple by-products, excess, troublesome separation and purification, etc.

Inactive Publication Date: 2021-03-30
HUBEI GRAND LIFE SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And in the process of generating ethambutol from D-2-aminobutanol and 1,2-dichloroethane, the more expensive D-2-aminobutanol needs a large excess to inhibit N-polyalkyl substitution reaction, even so, there will still be more by-products, which will cause trouble for separation and purification
Therefore, the existing method for preparing ethambutol hydrochloride also has many shortcomings, and it is necessary to find a new method with good selectivity, high yield, little environmental pollution, and easy operation

Method used

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  • Novel method for preparing ethambutol hydrochloride
  • Novel method for preparing ethambutol hydrochloride
  • Novel method for preparing ethambutol hydrochloride

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Effect test

Embodiment 1

[0019] Embodiment 1: the synthesis of L-2-aminobutyric acid

[0020] Add 2382.4g L-threonine (20mol), 1261.2g ammonium formate (1mol), 1L TD enzyme solution, 1L FDH / FDH co-expression crude enzyme solution, 2L NAD+ and The mixed solution of pyridoxal phosphate was reacted at 40°C for 24 hours. After the macroporous resin adsorbed macromolecular impurities, the product was concentrated, and ethanol was added to dissolve the impurities. The obtained solid product was filtered and dried for the next reaction. The dried product is 1959.2g of L-2-aminobutyric acid with a purity of 96%, and the yield is 91%.

Embodiment 2

[0021] Embodiment 2: the synthesis of diamide dicarboxylic acid

[0022] 200 milliliters of dichloromethane, 103.12 g of L-2-aminobutyric acid (1 mol), 76.16 g of oxalyl chloride (0.6 mol) and 200 milliliters of triethylamine were added to the reaction kettle, and at 100° C., the amidation reaction was carried out for 12 hours. Obtain (2S,2S')-N,N'-bis(2-butyric acid)-oxamide, that is, diamide dicarboxylic acid. After the reaction, the excess low-boiling point solvent was removed by rotary evaporation, and the remaining solid was recrystallized in an aqueous solution and dried to obtain 213.4 g of diamide dicarboxylic acid with a yield of 82%.

Embodiment 3

[0023] Embodiment 3: the synthesis of ethambutol

[0024] Add 1L methanol, 130.13g diamide dicarboxylic acid (0.5mol), catalyst 22.17g Co(BF4)2·6H2O (0.025mol) and equimolar amount of tridentate phosphine ligand 1,1,1-tri (Diphenylphosphinomethyl)ethane (15.62 g) was fed with hydrogen, the pressure was maintained at 0.5 MPa, and catalytic hydrogenation was carried out at 150° C. for 2 h to obtain 183.88 g of ethambutol with a yield of 90%.

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Abstract

According to the invention, cheap and easily available L-threonine is used as a raw material to synthesize L-2-aminobutyric acid, and then the L-2-aminobutyric acid is used as an intermediate to synthesize ethambutol hydrochloride. Firstly, an enzyme catalysis method is used, L-threonine is used as a raw material, and L-2-aminobutyric acid (D-2-aminobutanol and L-2-aminobutyric acid are both in Sconfiguration) is prepared through a 'one-pot method'; the intermediate reacts with oxalyl chloride to generate a dicarboxylic acid compound containing diamide groups, and then cobalt catalytic hydrogenation reduction is conducted to obtain ethambutol; and hydrogen chloride gas is introduced to generate ethambutol hydrochloride. The process has the characteristics of low cost, simplicity and convenience in operation, environmental friendliness, high conversion rate and high optical purity of the product.

Description

technical field [0001] The invention relates to a technology for preparing ethambutol hydrochloride. Background technique [0002] Tuberculosis is a chronic infectious disease that seriously endangers people's health. At present, there are about 2 billion people infected with tuberculosis in the world, and there are about 8.5 to 10 million new tuberculosis patients every year, and about 2.5 million deaths due to tuberculosis every year. China is one of the 22 countries with severe tuberculosis epidemics in the world, and it is also one of the 27 countries with severe multidrug-resistant tuberculosis epidemics in the world. The number of tuberculosis patients ranks second in the world, second only to India. The annual incidence of tuberculosis in China is about 1.4 million, and the number of deaths due to tuberculosis reaches 150,000 per year, exceeding the total number of deaths from other infectious diseases. Therefore, tuberculosis is one of the major diseases to be contr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P13/04C07C213/02C07C215/14C07C231/02C07C233/56
CPCC07C213/02C07C231/02C12P13/04C07C215/14C07C233/56
Inventor 孙华君刘年金江汝泳郭晨熊先胜钱志强
Owner HUBEI GRAND LIFE SCI & TECH CO LTD
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