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Alfacalcidol precursor preparation method

A technology of alphacalcidol and alfacalcidol, which is applied in the direction of organic chemistry, can solve the problems of large consumption of raw materials, long development cycle, high material cost, etc., and achieve low cost, improved utilization and simple preparation process Effect

Inactive Publication Date: 2020-02-28
CHONGQING MEDICAL & PHARMA COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The previous high-performance liquid chromatography with alfacalcidol as the reference substance can directly locate the position of its chromatographic peak, significantly reduce or eliminate the influence of relative retention time and UV response difference, and the content determination is more accurate, but this method requires high Pure pre-alfacalcidol as reference substance
[0004] Because pro-alfacalcidol is extremely unstable, it is prone to tautomerism with alfacalcidol at room temperature. If you want to directly synthesize pro-alfacalcidol, you need to design a synthetic route, which has a long development cycle and high cost. high, difficult
If pro-alfacalcidol is directly separated and prepared from the bulk drug, a large amount of bulk drug will be consumed, and there is also the problem of high material cost

Method used

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Effect test

Embodiment 1

[0020] A preparation method for pro-alphacalcidol, is characterized in that, comprises the following steps:

[0021] 1) The obtained alfacalcidol raw material is placed in a reactor (round bottom flask) and dissolved with absolute ethanol.

[0022] The raw material weight of alfacalcidol is 200 mg, and the volume of absolute ethanol is 100 mL.

[0023] 2) Heat the reactor described in step 1, heat it in a hot water bath at 80°C to condense and reflux for 2 hours.

[0024] 3) Take out the product in the reactor in step 2), and remove the ethanol by rotary evaporation under reduced pressure in a hot water bath at 60°C.

[0025] 4) Add mobile phase to dissolve the product obtained in step 3), that is, liquid phase preparation

[0026] The volume ratio of each component of the mobile phase is

[0027] 8 parts n-heptane

[0028] 9 parts ethyl acetate

[0029] 3 parts dichloromethane

[0030] The weight of the product obtained in step 3) is about 200mg, and the volume of the m...

Embodiment 2

[0035] A preparation method for pro-alphacalcidol, is characterized in that, comprises the following steps:

[0036] 1) The obtained alfacalcidol raw material is placed in a reactor (round bottom flask) and dissolved with absolute ethanol.

[0037] The raw material weight of alfacalcidol is 400mg, and the volume of absolute ethanol is 100mL.

[0038] 2) Heat the reactor described in step 1, heat in a hot water bath at 90°C, condense and reflux for 1.5 hours.

[0039] 3) Take out the product in the reactor in step 2), and remove the ethanol by rotary evaporation under reduced pressure in a hot water bath at 60°C.

[0040] 4) Add mobile phase to dissolve the product obtained in step 3), that is, liquid phase preparation

[0041] The volume ratio of each component of the mobile phase is

[0042] 8 parts n-heptane

[0043] 9 parts ethyl acetate

[0044] 3 parts dichloromethane

[0045] The weight of the product obtained in the step 3) is about 400mg, and the volume of the mo...

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Abstract

The invention provides an alfacalcidol precursor preparation method. According to the method, an alfacalcidol precursor is prepared through high-temperature water bath reflux, and is separated and purified through high performance liquid chromatography, the structure of the alfacalcidol precursor is identified through HRMS and NMR, and the result shows that the obtained compound is the alfacalcidol precursor. According to the invention, the method is simple in process, short in period, low in cost, high in yield and capable of achieving cyclic preparation.

Description

technical field [0001] The present invention relates to drug analysis experiments. Background technique [0002] Alphacalcidol chemical name: (5Z,7E)-9,10-cyclocholesta-5,7,10(19)-triene-1α,3β-diol. The mechanism of action is to avoid osteomalacia by regulating the utilization of calcium. Its active metabolites also regulate osteoblasts, produce important bone matrix proteins and growth factors, and are extremely important for bone renewal and repair of micro-fractures. Alfacalcidol tablets were launched in Japan in July 1988. The indications are osteoporosis, improvement of chronic renal failure, hypoparathyroidism, and resistance to vitamin D caused by rickets, osteomalacia and other diseases. Various symptoms of metabolic abnormalities. [0003] According to the relevant guidelines and document requirements, the consistency evaluation of self-made alfacalcidol tablets and the reference preparation was carried out in the pharmaceutical research, and it was found that th...

Claims

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Application Information

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IPC IPC(8): C07C401/00
CPCC07C401/00C07C2601/16C07C2602/24
Inventor 邱妍川张慧梅钟玲
Owner CHONGQING MEDICAL & PHARMA COLLEGE
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