A kind of preparation method of acicular methylene white crystal

A methylene white crystal technology, which is applied in the field of preparation of needle-like methylene white crystals, achieves the effects of low production cost, low toxicity, and prolonged residence time

Inactive Publication Date: 2015-11-11
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, the preparation method of generating methylene white crystals in solution has not been reported

Method used

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  • A kind of preparation method of acicular methylene white crystal
  • A kind of preparation method of acicular methylene white crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Prepare 45 ml of an aqueous solution containing 0.091 moles per liter of L-glutamic acid, 0.024 moles per liter of disodium hydrogen phosphate and 0.038 moles per liter of sodium hydroxide, stir at room temperature to dissolve completely; then add calcium nitrate and urea in sequence and methylene blue at concentrations of 0.026 moles per liter, 0.056 moles per liter and 0.696 millimoles per liter, respectively;

[0021] (2) Stir the solution in step (1) evenly and transfer it to a stainless steel autoclave with a charging rate of 90%, react at a temperature of 100oC for 24 hours, then heat up to 160oC for 24 hours and then cool to room temperature;

[0022] (3) The reaction product obtained in step (2) was filtered and washed to prepare needle-like methylene white crystals, and finally put into 25 ml of an aqueous solution containing 0.381 moles per liter of sodium sulfite for sealed storage.

[0023] Optical microscope inspection product morphology see figure 1 ....

Embodiment 2

[0025] (1) Prepare 45 ml of an aqueous solution containing 0.091 moles per liter of L-glutamic acid, 0.024 moles per liter of disodium hydrogen phosphate and 0.038 moles per liter of sodium hydroxide, stir at room temperature to completely dissolve, then add calcium nitrate and urea in sequence and methylene blue at concentrations of 0.026 moles per liter, 0.056 moles per liter and 0.696 millimoles per liter, respectively;

[0026] (2) Stir the solution in step (1) evenly and transfer it to a stainless steel autoclave with a charging rate of 90%, treat it at 100oC for 24 hours, then heat it up to 140oC for 24 hours and cool to room temperature;

[0027] (3) The reaction product obtained in step (2) was filtered and washed to prepare needle-like methylene white crystals, and finally put into 25 ml of an aqueous solution containing 0.762 moles per liter of sodium sulfite for sealed storage.

[0028] Optical microscope inspection product morphology see figure 2 .

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Abstract

The invention provides a preparation method of acicular methylene white crystals, belonging to the technical field of chemical raw material production. The method comprises the steps of firstly, adding L-glutamic acid, disodium hydrogen phosphate and sodium hydroxide into an aqueous solution; after the added objects are completely dissolved, adding urea, calcium nitrate and methylene blue; after the obtained solution is uniformly stirred, transferring the obtained product to a high-pressure reaction kettle, wherein the loading rate of the high-pressure reaction kettle is 90%; then, reacting for 24 hours at the temperature of 100 DEG C, reacting for 24 hours at the temperature of 140-160 DEG C, cooling to room temperature, and filtering and washing the obtained product, so that a reduced-state product of methylene blue, namely methylene white crystal can be obtained; finally, putting the methylene white crystal into an aqueous solution containing a reducing agent to be sealed and stored, wherein the length of the crystal is 0.2-8 mm. The method is simple in process, low in raw material price, and easy for industrial production.

Description

technical field [0001] The invention provides a method for preparing acicular methylene white crystals, which belongs to the technical field of chemical raw material production. Background technique [0002] Methylene blue has been widely used in the treatment of diseases such as malaria, methemoglobinemia and urinary tract infection, and it has been found in clinical trials that methylene blue has a significant inhibitory effect on the aggregation of tall proteins in patients with Alzheimer's disease. However, as an oral drug, methylene blue needs to be reduced to methylene white by reductase in the stomach before it can enter the human blood and be absorbed in order to achieve its therapeutic effect. Due to the limitation of the residence time of the drug in the stomach, usually only part of the methylene blue is reduced in the stomach. After the stomach is emptied, the methylene blue is transported to the alkaline environment of the small intestine and other organs and ea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D279/20
CPCC07D279/20
Inventor 葛筱璐李成峰
Owner SHANDONG UNIV OF TECH
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