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Synthetic method of long-acting sulfonamide

A synthetic method and long-acting sulfonamide technology, applied in the direction of organic chemistry to achieve the effect of increasing yield and reducing cost

Active Publication Date: 2015-11-18
SUZHOU WUGAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, still lack a kind of synthetic method of the long-acting sulfonamide of high yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0012] The synthesis method of the long-acting sulfonamide of the present invention comprises the following steps: (a) sequentially adding methanol, caustic soda and sulfachloropyridazine sodium into the reaction kettle, stirring and reacting at 0.1~1.0MPa and 50~160°C for 1 After ~15 hours, the first mixed solution is obtained, and the reaction kettle is lowered to normal temperature and normal pressure (normal temperature is 10-30°C, and normal pressure is atmospheric pressure); the methanol, the caustic soda and the sulfachloropyridazine The mass ratio of sodium is 1~3:0.1~0.8:1; the caustic soda is sodium hydroxide, potassium hydroxide, lithium hydroxide, sodium methylate, potassium methylate or lithium methylate; (b) mixing the first After the liquid was evaporated to dryness, the first deionized water was added to dissolve, the pH value was adjusted to 5.4~6.3 to crystallize the product, and the crude product was obtained by suction filtration; the ratio of the methanol t...

Embodiment 1

[0016] The present embodiment provides a kind of synthetic method of long-acting sulfonamide, and it comprises the following steps:

[0017] (a) Check that the bottom valve of the autoclave is closed, open the vacuum valve, add 250g of methanol into the autoclave, slowly add 16g of sodium hydroxide (adding speed is about 10g / min) into the autoclave, and then put 100g sodium sulfachloropyridazine is put into the stuffy autoclave, and the feed opening and vacuum valve are closed.

[0018] (b) Start stirring and heat to 160°C. When the pressure in the kettle reaches 1.0MPa, keep the temperature and hold the pressure for 1 hour to obtain the first mixed liquid; then cool down to 10°C and atmospheric pressure, concentrate and recover methanol (the heating temperature is generally at 60 ~90°C, the higher the temperature, the easier it is to bump) until evaporated to dryness; add 150ml of deionized water, heat to dissolve (heating temperature is 40~70°C), then add hydrochloric acid d...

Embodiment 2

[0021] The present embodiment provides a kind of synthetic method of long-acting sulfonamide, and it comprises the following steps:

[0022] (a) Check that the bottom valve of the autoclave is closed, open the vacuum valve, add 200g of methanol into the autoclave, slowly add 10g of sodium hydroxide (adding speed is about 10g / min) into the autoclave, and then put 100g sodium sulfachloropyridazine is put into the stuffy autoclave, and the feed opening and vacuum valve are closed.

[0023] (b) Start stirring and heat to 50°C. When the pressure in the kettle reaches 0.1MPa, heat and hold the pressure for 15 hours to obtain the first mixed liquid; then cool down to 25°C and atmospheric pressure, concentrate and recover methanol (the heating temperature is generally at 60 ~90°C, the higher the temperature, the easier it is to bump) until evaporated to dryness; add 180ml of deionized water, heat to dissolve (heating temperature is 40~70°C), then add hydrochloric acid dropwise to adju...

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PUM

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Abstract

The invention relates to a synthetic method of long-acting sulfonamide. The synthetic method comprises the following steps: (a) sequentially adding methyl alcohol, caustic soda flakes and sulfachloropyridazine sodium into a reaction kettle, stirring for reaction for 1-15 hours at the pressure of 0.1-1.0 MPa and the temperature of 50-160 DEG C to obtain a first mixed solution, cooling the reaction kettle to a normal temperature, and depressurizing the reaction kettle to normal pressure, wherein the mass ratio of the methyl alcohol to the caustic soda flakes to the sulfachloropyridazine sodium is (1-3): (0.1-0.8): 1; (b) evaporating the first mixed solution to dryness, adding first deionized water for dissolution, adjusting the pH value to be 5.4-6.3 for product crystal precipitation, and carrying out suction filtration to obtain a crude product, wherein the ratio of the methyl alcohol to the first deionized water is (2-3) g: (1.5-2) ml; (c) adding the crude product into a decoloration 3-mouth bottle, adding second deionized water for dissolution, adjusting the pH value to be 12-14, adding activated carbon, stirring for 10-60 minutes at the temperature of 0-100 DEG C, filtering, adjusting the pH of the filtrate to be 5.4-6.3 for product crystal precipitation, carrying out suction filtration, and drying, wherein the ratio of the methyl alcohol to the second deionized water to the activated carbon is (2-3) g: (4-6) ml: (0.05-0.2) g. According to the synthetic method, the yield of the long-acting sulfonamide can be improved, and the cost is reduced.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a synthesis method of long-acting sulfonamide. Background technique [0002] Sulfonamides are a relatively commonly used class of drugs. They have a broad antibacterial spectrum, can be taken orally, and are absorbed quickly. Some (such as sulfadiazine, SD) can penetrate into the cerebrospinal fluid through the blood-brain barrier, are relatively stable, and are not easy to deteriorate. Long-acting sulfonamide is a special sulfa drug, also known as 4-amino-N-(6-methoxypyridazin-3-yl) benzenesulfonamide sodium, the structural formula is . [0003] The Chinese Invention Patent No. 201010294636.3 discloses a method for preparing long-acting sulfa drugs, adding sulfa-6-methoxine anhydrous to a solvent system composed of propanol and water, adding alkaline solution to adjust the solution The pH value is 8~12, then stirred in a water bath with a temperature of 30~50°C fo...

Claims

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Application Information

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IPC IPC(8): C07D237/22
CPCC07D237/22
Inventor 吴水亮
Owner SUZHOU WUGAN PHARMA
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