Preparation method of calcitriol
A technology for calcitriol and compound, which is applied in the field of preparation of compound raw material calcitriol, can solve the problems of unsuitable separation of calcitriol, high impurities in the separation result and high analysis cost, and saves time for separation and preparation , the method selection is reasonable, the effect of the efficient preparation method
A technology for calcitriol and compound, which is applied in the field of preparation of compound raw material calcitriol, can solve the problems of unsuitable separation of calcitriol, high impurities in the separation result and high analysis cost, and saves time for separation and preparation , the method selection is reasonable, the effect of the efficient preparation method
CN101607931AActive Publication Date: 2009-12-23CP PHARMA QINGDAO CO LTD
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[0023] The main process involved in this embodiment is the same as in the summary of the invention, wherein the three specific processes of the separation and preparation of compound 3a, the separation and preparation of compound 4a and the separation and preparation of compound 5a are as follows:
[0024]
[0025] Add compound 2a and sodium bicarbonate to methanol in turn, stir and maintain the temperature at 30ยฐC, and use thin-layer chromatography (thin-layer chromatography conditions: silica gel is GF254; developing solvent: ethyl acetate-cyclohexane 3:1; The color agent is 5% phosphomolybdic acid or ethanol) to detect the degree of progress of the reaction; after the reaction is substantially complete, the methanol is recovered under reduced pressure and extracted with ethyl acetate, after drying and concentrating, the medium-pressure liquid chromatography column is used, and the mobile phase is ethyl acetate : Cyclohexane 1: 20, the flow rate is 10ml / min for elution, th...
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The invention relates to a preparation method of calcitriol which is a compound material, belonging to the technical field of preparation of drug synthesis and organic compound synthesis. In the invention, the calcifediol is taken as raw material, a majority of produced impurities in the chemical reaction process are removed through medium-pressure liquid phase chromatography, wherein calcifediol carried out sulfonylation and ring closing on toluene, and the medium-pressure liquid phase chromatography is used for removing the impurities; products carry out oxidation reaction, medium-pressure chromatographic column separates and removes the impurities, ring opening is carried out, medium-pressure liquid phase is added for coarsely separating stereoisomeride, and at last the products separated by high-pressure liquid phase chromatography is hydrolyzed and refined to obtain the calcitriol. The invention is reasonably selected, comprehensively applies the advantages of the medium and high pressure liquid phase chromatography, has simple detaching method, can effectively remove the impurities, thoroughly separates the stereoisomeride, has high purity of the calcitriol obtained from separation, has a productive rate of 40 percent, high yield and low cost, shortens production period, is suitable for industrial scale, has application prospect, and provides a time-saving, economic and efficient method for the separation and the preparation of chiral compounds.
Description
Technical field: [0001] The invention relates to a method for preparing a compound raw material calcitriol, which belongs to the technical field of drug synthesis and organic compound synthesis and preparation. Background technique: [0002] Calcitriol, chemical name: 9,10-cyclocholesta-5Z,7E,10(19)-triene-1ฮฑ,3ฮฒ,25-triol. The chemical formula is: [0003] Calcitriol is a drug with multiple chiral centers, a fat-soluble sterol in vitamin D compounds, and a class of substances involved in the stability of the internal environment of calcium and phosphorus and the mineralization of bone. Calcitriol is Vitamin D 3 Active vitamin D converted in the body by 25-hydroxylase in the liver and 1ฮฑ-hydroxylase in the kidney. Calcitriol can treat postmenopausal women and middle-aged and elderly osteoporosis, hypoparathyroidism, vitamin D 3 Dependent rickets, renal osteodystrophy, and renal rickets, renal bone lesions, and hypoparathyroidism caused by renal failure and other kidney d...
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Patent Timeline
23 Dec 2009
Publication
CN101607931A
- IPC
- C07C401/00; B01D15/08; A61P19/10; A61P5/18; A61P13/12; A61P35/00
- Inventors
- ็ๆๅ; ไปป่