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Synthetic method of chromium picolinate

A kind of technology of chromium picolinate and synthesis method, applied in directions such as organic chemistry, to achieve the effects of good crystal form, high purity and easy control of technological process

Active Publication Date: 2014-06-04
河北富格药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Aiming at the problems existing in the existing chromium picolinate synthesis process, the invention provides a synthetic method for chromium picolinate

Method used

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  • Synthetic method of chromium picolinate

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Experimental program
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Effect test

Embodiment 1

[0026] 2-cyanopyridine hydrolysis

[0027] Add 0.05 mol of weighed 2-cyanopyridine into 50ml of ethanol and stir to dissolve, heat up to 78°C, then add 10ml of NaOH aqueous solution with a mass concentration of 30%, and react for 1 hour to detect 2-cyanopyridine by high performance liquid chromatography After the conversion is complete, add 20ml of water, control the temperature to 70°C, and then add hydrochloric acid to adjust the pH to 8-9;

[0028] complexation reaction

[0029] Control the temperature to 70°C, add dropwise 41.5ml of chromium potassium sulfate aqueous solution with a mass concentration of 20% to the above hydrolyzate while stirring continuously, after 1h dropwise addition, continue to stir for 2h, then cool down to 25°C and suction filter, filter The material was washed with 30ml of purified water and then washed with 30ml of ethanol, and then the filtered material was dried at 60°C to obtain 6.62g of chromium picolinate, with a yield of 95%. The purity of...

Embodiment 2

[0031] 2-cyanopyridine hydrolysis

[0032] Add 0.05 mol of weighed 2-cyanopyridine into 75ml of ethanol and stir to dissolve, then raise the temperature to 78°C, then add 14ml of NaOH aqueous solution with a mass concentration of 30%, and react for 1 hour to detect 2-cyanopyridine by high performance liquid chromatography After the transformation has been completed, add 16ml of water, control the temperature to 70°C, and then add hydrochloric acid to adjust the pH to 8-9;

[0033] complexation reaction

[0034] Control the temperature to 60°C, add dropwise 42.6ml of chromium potassium sulfate aqueous solution with a mass concentration of 20% to the above hydrolyzate while stirring continuously, after 1h dropwise addition, continue to stir for 2h, then cool down to 25°C and suction filter, filter The material was washed with 30ml of purified water and then washed with 30ml of ethanol, and then dried at 60°C to obtain 6.48g of chromium picolinate, with a yield of 92.9%. The pur...

Embodiment 3

[0036] 2-cyanopyridine hydrolysis

[0037]Add 0.05 mol of weighed 2-cyanopyridine into 50ml of methanol, stir and dissolve, heat up to 65°C, then add 10ml of NaOH aqueous solution with a mass concentration of 30%, and react for 1 hour to detect 2-cyanopyridine by high performance liquid chromatography After the conversion is complete, add 20ml of water, control the temperature to 70°C, then add concentrated hydrochloric acid to adjust the pH to 8-9;

[0038] complexation reaction

[0039] Control the temperature to 70°C, add dropwise 41.5ml of chromium potassium sulfate solution with a mass concentration of 20% to the above hydrolyzate while stirring continuously, after 1h of dropwise addition, continue to stir for 2h, then cool down to 25°C and suction filter, filter The material was washed with 30ml of purified water and then washed with 30ml of ethanol, and then the filtered material was dried at 60°C to obtain 6.27g of chromium picolinate, with a yield of 90.1%. The purit...

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Abstract

The invention discloses a synthetic method of chromium picolinate; the method comprises the steps of: adding 2-cyanopyridine into methanol or ethanol for dissolution, and then adding NaOH or KOH water solution; reacting for 1 hour, adding water and controlling temperature, adjusting pH value to 8-9; dropping potassium chromium sulfate water solution at 50-70 DEG C; stirring, cooling and pumping filtrating, and washing and drying filtered products so as to obtain the chromium picolinate. Because the 2-cyanopyridine is resolved in homogeneous for reaction, so only one hour is needed for hydrolyzation, thereby greatly reducing reaction time; the product is in rose color, good in fluidity, crystal form is hexagon; because complexation reaction employs chromic salt potassium chromium sulfate, so the obtained chromium picolinate is high in purity; the purity can reach 99.8% and above, and total impurity is smaller than 0.5%, thereby solving high energy consumption, high danger and high production equipment requirement problems caused by high temperature and high pressure reaction, and removing safety troubles brought by usage of sodium dichromate; the method is short in technology reaction time, simple in process, technology process is easy to control, production yield is high, crystal form is good and purity is high, and industrialization production can be realized.

Description

technical field [0001] The present invention relates to the synthetic method of chromium picolinate. Background technique [0002] Chromium picolinate is a complementary or alternative drug used in type 2 diabetes, and studies have shown that chromium picolinate can significantly improve insulin sensitivity in diabetic patients. In August 2005, the US Food and Drug Administration approved the production of chromium picolinate and confirmed that it can be safely used in the treatment of human insulin resistance and type Ⅱ diabetes. In my country's health care product market, chromium picolinate has been allowed to be added to health food. [0003] At present, the synthesis techniques of chromium picolinate mainly include the following: US5677461 reported that 0.019mol of chromium chloride and 0.058mol of 2-picolinate were dissolved in 30ml of water, and the pH was adjusted to 3.8 with NaOH, and heated to 70°C for 10 minutes. , cooling and suction filtration to obtain 0.017m...

Claims

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Application Information

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IPC IPC(8): C07D213/803C07D213/79
CPCC07D213/79C07D213/803
Inventor 岳振路
Owner 河北富格药业有限公司