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High-purity seed cycling injection method for recrytallizing methyclothiazide

A technology of methylchlorothiazide and recrystallization, which is applied in the field of refining and purification of pharmaceutical chemical raw materials, can solve the problems of low recrystallization yield, solvent waste, and low production efficiency, and achieve the improvement of raw material utilization efficiency, increase yield, and increase production efficiency effect

Active Publication Date: 2015-01-21
CHANGCHUN MAILING BIOLOGICAL ENG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to provide a high-purity seed circulation injection method for methylchlorothiazide recrystallization, to solve the problems of low recrystallization yield of methylchlorothiazide in a crystallization solvent, solvent waste, and low production efficiency

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Calculation of Feed Amount of Recrystallization Sample

[0036] 310g (m) of methylchlorothiazide raw material is recrystallized once, divided into 4 sub-batches (n) for recrystallization, then the first sub-batch of recrystallization feeding amount (x) is:

[0037] x+(n-1)×0.7x=m

[0038] x+(4-1)×0.7x=310g

[0039] x+2.1x=310g

[0040] 3.1x=310g

[0041] x=100g

[0042] The 2nd, 3rd, 4th sub-batches feed amount is: 0.7x=70g

[0043] Calculated according to the formula, the feeding amount between each sub-batch of methylchlorothiazide raw material can be obtained as 100g: 70g: 70g: 70g.

[0044] Operation method: Divide 310g of Meclothiazine raw material into 4 sub-batches for one-time crystallization, calculate according to the formula that the feeding amount of the first sub-batch is 100g, and the feeding amount of the remaining 2nd, 3rd, and 4th sub-batches is 70g, a total of 310g, Weigh 10...

Embodiment 2

[0049]Recrystallize 7.5 kg of methylchlorothiazide raw material twice, the first recrystallization is divided into 4 sub-batches, and the second recrystallization is divided into 3 sub-batches.

[0050] The first recrystallization: The first recrystallization is divided into four sub-batches, and the 2nd, 3rd, and 4th sub-batches are all 0.7 times of the 1st sub-batch, and the calculation of the 1st sub-batch (x) is as follows Formula calculation: x+(number of sub-batches-1)×0.7x=total amount of samples to be recrystallized

[0051] x+(n-1)×0.7x=m

[0052] x+(4-1)×0.7x=7.5㎏

[0053] x+2.1x=7.5㎏

[0054] 3.1x=7.5kg

[0055] x≈2.4㎏ 0.7x≈1.7㎏

[0056] The feeding amount of the first sub-batch of the first recrystallization is 2.4kg, and the feeding amount of the second, third, and fourth sub-batches is 1.7kg each

[0057] Operation method: Weigh 2.4 kg of methylchlorothiazide raw material, put it in a 150L reaction ke...

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Abstract

The invention discloses a high-purity seed cycling injection method for recrytallizing methyclothiazide. High-purity seeds can be circularly injected for 1 to 4 times to be recrytallized and extracted. The invention particularly relates to a method for recrystallizing methyclothiazide in methanol. The mass ratio of a methyclothiazide raw material and the methanol is 1:30, the inventory ratio of a first sublot and each sublot is 1:0.7, a first sublot crystallizing mother solution can be used as a seed to use mechanically by the recrystallization of a next sublot, the seeds produced by the previous sublot of each recrystallization is only used mechanically by the recrystallization of a next sublot, the seed is only used mechanically by the sublots of the same recraystallization, the methyclothiazide raw material is recrystallized by circularly injecting the seeds, so that the recrystallization yield of the methyclothiazide is greatly increased, the consumption of the crystallization solvent is saved, the production efficiency is improved, and the yield is greatly improved by 10 to 30 percent compared with one-time recrystallization and simple mechanical use of the mother solution.

Description

technical field [0001] The invention belongs to the field of refining and purifying medicinal chemical raw materials, in particular to a high-purity seed circulation injection method for methylchlorothiazide recrystallization, which is a purification method for methylchlorothiazide recrystallization by using the high-purity seed circulation injection technology. Background technique [0002] Methylchlorothiazide is an oral thiazide diuretic, which can effectively lower blood pressure, reduce the risk of stroke and other cardiovascular diseases, and is an orally effective diuretic and antihypertensive drug. [0003] Methylchlorothiazide is white crystalline powder, odorless; this product is dissolved in acetone or 0.1mol / L sodium hydroxide solution, slightly soluble in methanol or ethanol, and dissolved in water, 0.1mol / L hydrochloric acid solution or chloroform insoluble. [0004] The purity of pharmaceutical-grade methylchlorothiazide raw materials can generally reach more...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D285/30
Inventor 于洪年杜宏明武杰高强张万顺
Owner CHANGCHUN MAILING BIOLOGICAL ENG CO LTD