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Synthetic method for repaglinide

A synthesis method and technology of mixed solution, applied in the field of repaglinide synthesis, can solve the problems of long synthesis time, low synthesis purity, solid residue and the like, and achieve the effects of short reaction time, improved reaction rate and stable quality

Inactive Publication Date: 2018-06-08
陈益德
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing repaglinide synthesis method, there is still a small amount of solid remaining in the solution, which is difficult to filter out, resulting in low synthesis purity and long synthesis time, which is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A kind of synthetic method of repaglinide, the concrete steps of this method are as follows:

[0018] S1: add 50 g of magnesium scraps and 2 g of iodine to 200 ml of tetrahydrofuran solution, add 15 g of isobutyl bromide at 20°C under nitrogen flow, and stir to react to obtain a reaction solution. The temperature of ℃, and the time of stirring reaction is 15min;

[0019] S2: Heat the toluene solution to 10°C, add the mixed solution, stir at the same temperature for 3 hours, stand for stratification, wash the organic layer with saturated sodium bicarbonate and water, and evaporate the solvent under reduced pressure to obtain a colorless liquid. The mixed solution It is a mixture of concentrated hydrochloric acid and ice water;

[0020] S3: mixing the reaction solution in step S1 into the colorless liquid, stirring at room temperature, then adding methanol 60ml and sodium hydroxide 2g, heating up and stirring, the temperature of heating and stirring is 50 ℃, and the stir...

Embodiment 2

[0024] A kind of synthetic method of repaglinide, the concrete steps of this method are as follows:

[0025] S1: add 70 g of magnesium scraps and 4 g of iodine to 300 ml of tetrahydrofuran solution, add 20 g of isobutyl bromide at 30°C under nitrogen flow, and stir to react to obtain a reaction solution, which is placed for later use. During the stirring reaction, keep 30 g The temperature of ℃, and the time of stirring reaction is 20min;

[0026] S2: Heat the toluene solution to 20°C, add the mixed solution, stir at the same temperature for 4 hours, stand for stratification, wash the organic layer with saturated sodium bicarbonate and water, and evaporate the solvent under reduced pressure to obtain a colorless liquid. The mixed solution It is a mixture of concentrated hydrochloric acid and ice water;

[0027] S3: mix the reaction solution in step S1 into the colorless liquid, stir at room temperature, then add 80 ml of methanol and 4 g of sodium hydroxide, heat up and stir ...

Embodiment 3

[0031] A kind of synthetic method of repaglinide, the concrete steps of this method are as follows:

[0032] S1: add 60 g of magnesium scraps and 3 g of iodine to 260 ml of tetrahydrofuran solution, add 18 g of isobutyl bromide at 25°C under nitrogen flow, and stir to react to obtain a reaction solution, which is placed for later use. During the stirring reaction, keep 25 The temperature of ℃, and the time of stirring reaction is 18min;

[0033] S2: heat the toluene solution to 15°C, add the mixed solution, stir at the same temperature for 3 hours, stand for stratification, wash the organic layer with saturated sodium bicarbonate and water, and evaporate the solvent under reduced pressure to obtain a colorless liquid. The mixed solution It is a mixture of concentrated hydrochloric acid and ice water;

[0034] S3: mixing the reaction solution in step S1 into the colorless liquid, stirring at room temperature, then adding 70 ml of methanol and 3 g of sodium hydroxide, heating u...

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PUM

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Abstract

The invention discloses a synthetic method for repaglinide, belonging to the technical field of chemical synthesis. The method comprises the following concrete steps: S1, obtaining a reaction solution, and carrying out standing for subsequent usage; S2, heating a toluene solution to 10 to 20 DEG C, and adding a mixed solution so as to obtain a colorless liquid; S3, mixing the reaction solution obtained in the step S1 with the colorless liquid, carrying out stirring at a room temperature, then adding 60 to 80 ml of methanol and 2 to 4 g of sodium hydroxide, and carrying out heating and uniformmixing under stirring; S4, adding 3 to 6 g of a catalyst, and allowing the catalyst to participate a reaction; and S5, after completion of the reaction, carrying out pressurizing so as to recycle an organic solvent, adjusting a pH value of an obtained material to 6 to 7 by using a hydrochloric acid solution with a concentration of 5%, carrying out cooling crystallization, and carrying out vacuum filtering, washing and drying so as to obtain white solid repaglinide. The synthetic method provided by the invention can shorten the integral time of the reaction, improves the rate of the reaction, is controllable for factors in the process of the reaction, can guarantee stable quality of a reaction product, and has the advantages of mild reaction conditions, short reaction time, simple process and applicability to industrialized production.

Description

technical field [0001] The invention discloses a method for synthesizing repaglinide, in particular to the technical field of chemical synthesis. Background technique [0002] Repaglinide is a novel non-sulfonylurea short-acting oral insulin secretion-stimulating hypoglycemic agent. Stimulation of insulin release from the pancreas results in a rapid reduction in blood glucose levels, which is dependent on functioning beta cells in the islets. It is different from other oral insulin-stimulating hypoglycemic agents in that it binds to different receptors to close APT-dependent potassium channels in the β-cell membrane, depolarize the β-cell, open the calcium channel, and increase the influx of calcium. Induce insulin secretion from β cells, and this product promotes insulin secretion faster than sulfonamides. In the existing repaglinide synthesis method, there is still a small amount of solid remaining in the solution, which is difficult to filter out, resulting in lower syn...

Claims

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Application Information

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IPC IPC(8): C07D295/135
CPCC07D295/135
Inventor 陈益德
Owner 陈益德
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