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Synthetic method of guanethidine subplate drug intermediate cycloheptanone

A technology of guanethidine sulfate and its synthesis method, which is applied in the field of synthesis of cycloheptanone, a pharmaceutical intermediate of guanethidine sulfate, can solve the problems of slow onset of action, reduce intermediate links, reduce reaction temperature and reaction time, The effect of increasing the reaction yield

Inactive Publication Date: 2016-04-06
CHENGDU ZHONGHENG HUATIE TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Guanethidine sulfate is used as an antihypertensive drug. After oral administration, the onset of effect is slow, and the antihypertensive effect reaches its peak in 3 to 4 days. The effect is strong and long-lasting

Method used

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  • Synthetic method of guanethidine subplate drug intermediate cycloheptanone

Examples

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Effect test

example 1

[0012] (i) In a reaction vessel equipped with a stirrer, a thermometer, and a dropping funnel, add 500ml of water, 1.5mol of aluminum powder, and a phosphoric acid solution with a mass fraction of 40%, so that the temperature of the solution is controlled at 60°C, and dropwise add nitromethyl Cycloethanol 1.2mol, after adding, keep the solution temperature at 40°C, add 30mL sulfuric acid solution with a mass fraction of 40% every 30min, add 3 times in total, keep the pH of the solution at 3 for 1h, then filter, the filtrate is aminomethyl Cycloethanoic aluminum sulfate solution, the filtrate cake is used for the next batch after being washed with solvent methanol;

[0013] (ii) Use sulfuric acid to adjust the pH of the solution to 2 °C, slowly add 1.5 mol of sodium sulfite dissolved in 200 ml of water to form a solution, control the reaction temperature at 3 °C, keep the constant temperature for 20 minutes after adding, and then raise the temperature to 30 ℃, the reaction time...

example 2

[0015] (i) In a reaction vessel equipped with a stirrer, a thermometer, and a dropping funnel, add 550 ml of water, 1.5 mol of metal zinc powder, and a phosphoric acid solution with a mass fraction of 45%, so that the temperature of the solution is controlled at 65° C. Cycloethanol 1.2mol, after the addition, keep the solution temperature at 45°C, add 30mL of sulfuric acid solution with a mass fraction of 43% every 30min, add 3 times in total, keep the pH of the solution at 3 for 1h, then filter, the filtrate is ammonia Cycloethanoic zinc sulfate solution, the filtrate cake is used for the next batch after being washed with methyl ether solvent;

[0016] (ii) Use sulfuric acid to adjust the pH of the solution to 3, reduce the temperature of the solution to 4°C, slowly add 1.7mol of sodium sulfite dissolved in 200ml of water to form a solution, control the reaction temperature at 4°C, keep the constant temperature state for 20 minutes after adding, and then raise the temperature...

example 3

[0018] (i) In a reaction vessel equipped with a stirrer, a thermometer, and a dropping funnel, add 600ml of water, 1.5mol of metal aluminum powder, and a phosphoric acid solution with a mass fraction of 50%, so that the temperature of the solution is controlled at 70°C, and dropwise add nitrate Cycloethanol 1.2mol, after the addition, keep the solution temperature at 50°C, add 30mL sulfuric acid solution with a mass fraction of 45% every 30min, add 3 times in total, keep the pH of the solution at 4 for 1h, then filter, the filtrate is ammonia Cycloethanoic aluminum sulfate solution, the filtrate cake is used for the next batch after washing with methanol solvent;

[0019] (ii) Use sulfuric acid to adjust the pH of the solution to 3, reduce the temperature of the solution to 5°C, slowly add 2mol of sodium sulfite dissolved in 200ml of water to form a solution, control the reaction temperature at 5°C, keep the constant temperature state for 20 minutes after adding, and then raise...

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Abstract

The invention provides a synthetic method of guanethidine subplate drug intermediate cycloheptanone. The synthetic method comprises the following steps: (1) adding 500 to 600ml of water, 1.5mol of metal powder, a phosphoric acid solution with the mass fraction of 40 to 50 percent into a reaction vessel provided with a stirrer, a thermometer and a dropping funnel, wherein the solution temperature is controlled to be 60 to 70 DEG C, dropwise adding 1.2mol of nitromethylcycloheanol, after adding, maintaining the solution temperature at 40 to 50 DEG C, adding 30mL of sulfuric acid solution with the mass fraction of 40 to 45 percent for 3 times every 30min, and maintaining the solution pH at 3 to 4 for 1h, wherein filter liquor is aminomethlcycloheanol sulfate liquor, and a filter liquor cake is used for the next batch after being washed by using a solvent; (2) regulating the solution pH to 2 to 3 by using sulfuric acid, reducing the solution temperature to 2 to 5 DEG C, slowly adding and dissolving 1.5 to 2mol of sodium sulfite in 200ml of water, then heating up to 30 to 35 DEG C, distilling by using steam till a non-oily matter is distilled off, separating out an oil layer, extracting a water layer for 10 to 15 times by a solvent, combining the oil layer and a solvent layer, distilling off the solvent at normal pressure, then performing reduced pressure distillation, and collecting 65 to 70 DEG C cut fraction to obtain the cycloheptanone.

Description

technical field [0001] The invention relates to a method for synthesizing cycloheptanone, a pharmaceutical intermediate of guanethidine sulfate. Background technique [0002] Guanethidine sulfate is used as an antihypertensive drug. After oral administration, the onset of effect is slow, and the antihypertensive effect reaches its peak in 3 to 4 days. The effect is strong and long-lasting. When the blood pressure is lowered, the heart rate is slowed down, the cardiac output is reduced, and the pulse pressure is reduced. Intravenous injection of large doses begins to excrete more norepinephrine and prevents reabsorption of vesicles, causing blood pressure to rise. Chronic administration begins to lower blood pressure due to the inability to release transmitters. Long-term medication replaces the transmitter stored in the vesicle and releases the transmitter, and then prevents the uptake and synthesis of the transmitter, so that the transmitter is exhausted and blood pressur...

Claims

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Application Information

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IPC IPC(8): C07C45/00C07C49/413C07C49/403C07C45/78
CPCC07C45/00C07C45/78C07C209/34
Inventor 彭响亮
Owner CHENGDU ZHONGHENG HUATIE TECH CO LTD
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