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Green method for synthesizing AE-active ester through microwave-assisted process

A microwave-assisted, green process technology, applied in the direction of organic chemistry, can solve the problems of many solvents, long reaction time, and low yield, and achieve the effects of low cost, simple operation, and high product purity

Inactive Publication Date: 2018-12-21
SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But this synthetic method reaction time is long, yield is low, and solvent is many

Method used

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  • Green method for synthesizing AE-active ester through microwave-assisted process

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Experimental program
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Effect test

Embodiment 1

[0031] The green process for the synthesis of AE-active ester by the microwave-assisted method comprises the following steps:

[0032] Add 30g of aminothioxamic acid and 50g of DM into 350mL of dichloromethane-acetonitrile mixture at 21-23°C, add 7.2mL of triethylamine and 0.4mL of pyridine, cool down to 16.5-18°C, add 23mL of triethyl phosphite dropwise, and add dropwise for 1h , using a microwave reactor, adjust the microwave holding temperature to 17°C, the microwave radiation power to 80W, the radiation time to 60min, and the stirring speed to 100 rpm. Cool down to below 10°C and filter with suction to obtain the crude product. Soak and wash the crude product in 150 mL of methanol at 22-24°C for 1 h to obtain 50.8 g of refined AE-active ester. Yield 97%, purity 99.1%.

Embodiment 2

[0034] The green process for the synthesis of AE-active ester by the microwave-assisted method comprises the following steps:

[0035] Add 30g of aminothioxamic acid and 50gDM into 350mL of dichloromethane-acetonitrile mixture at 21-23°C, add 10mL of triethylamine and 3mL of aniline, cool down to 15.5-17°C, add 23.5mL of triethyl phosphite dropwise, add dropwise for 1.5h , using a microwave reactor, adjust the microwave holding temperature to 20°C, the microwave radiation power to 150W, the radiation time to 40min, and the stirring speed to 200 rpm. Cool down to below 10°C and filter with suction to obtain the crude product. The crude product was soaked in 150 mL of methanol at 22-24°C for 1 h to obtain 49.8 g of refined AE-active ester. Yield 95%, purity 99.2%.

Embodiment 3

[0037] The green process for the synthesis of AE-active ester by the microwave-assisted method comprises the following steps:

[0038] Add 30g of aminothioxamic acid and 50gDM to 350mL of dichloromethane-acetonitrile mother liquor at 22°C, add 4mL of pyridine and 0.4mL of aniline, cool down to 18°C, add 23mL of triethyl phosphite dropwise, add dropwise for 1h40min, use a microwave reactor, adjust the microwave The heat preservation temperature is 25°C, the microwave radiation power is 200W, the radiation time is 30min, and the stirring speed is 50 rpm. Cool down to below 10°C and filter with suction to obtain the crude product. The crude product was soaked in 150 mL of methanol at 22-24°C for 1 h to obtain 49.8 g of refined AE-active ester. Yield 95%, purity 99.1%.

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Abstract

The invention belongs to the technical field of synthesis of medicines and particularly relates to a green method for synthesizing AE-active ester through a microwave-assisted process. The green method for synthesizing AE-active ester through the microwave-assisted process comprises the following steps: firstly adding 2-(2-aminothiazole-4-yl)-2-methoxyiminoacetic acid, dithiodibenzothiazole, catalyst and solvent into a microwave reactor, then dropwise adding triethyl phosphate into the microwave reactor, reacting, carrying out suction filtration and recrystallization to obtain a product. The synthesis method is simple to operate and low in cost; the productivity can be greatly improved; the yield is increased and reaches up to 95%; the purity of the product is relatively high and reaches over 99%; the pleasantly surprised technical effect can be obtained.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical synthesis, and in particular relates to a green process for synthesizing AE-active ester with microwave assistance. Background technique [0002] Microwave chemistry is a new interdisciplinary subject developed vigorously in the 1990s. Its content is mainly to use high-frequency microwave energy to change the positive and negative poles of dipole molecules in reactants and solvents at a speed of billions of times per second. , produce dipole eddy current, ion conduction and high-frequency friction, and generate a large amount of heat in a short time, thereby promoting various chemical reactions. At present, microwave heating technology is widely used in synthetic chemistry, analytical chemistry, petrochemical industry, mineral metallurgy and other chemical research. However, the severe thermal effect in the microwave heating process is easy to produce a series of side reactions. [0003] L...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/74
CPCC07D277/74
Inventor 房正薇孟宪强贾开磊于复刚
Owner SHANDONG JINCHENG KERUI CHEMICAL CO LTD