Preparation method for alfacalcidol

Abstract

The invention relates to a preparation method for a compound, in particular to the preparation method for separating and purifying alfacalcidol. Aiming at the deficiencies of the conventional preparation technology, the invention provides a novel method for preparing alfacalcidol with good yield and high purity. The preparation method comprises the steps as follows: taking vitamin D3 as a raw material; removing most of trans-isomer impurities generated after chemical reaction by utilizing Diels-Alder reaction; and refining and purifying by preparative high pressure liquid chromatography to prepare high-purity alfacalcidol. According to the preparation method, the reaction conditions are moderate, the yield is high, and the purity of alfacalcidol reaches up to 99.5%.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a preparation method for the separation and purification of alfacalcidol, which belongs to the field of drug synthesis. (Technical Field of Organic Compound Synthesis) Background technique [0002] Alfacalcidol, chemical name: 9,10-cyclocholesta-5Z,7E,10(19)-triene-1a,3b-diol. The chemical formula is: [0003] [0004] Alfacalcidol is a fat-soluble sterol in vitamin D compounds, which is a kind of substance involved in the stability of the internal environment of calcium and phosphorus and the mineralization process of bone. Alfacalcidol is Vitamin D 3 Active vitamin D converted in the body by the action of 1α-hydroxylase in the kidneys. [0005] Alfacalcidol 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 caus...

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Problems solved by technology

Capillary electrophoresis has a good separation effect, and the separated product is clean, with little pollution and low cost, but its channel is thin, the separated samples are few, and alfacalcidol has no obvious positive and negative electrodes, so it is not suitable for the separation of alfacalcidol

Among planar chromatography, thin-layer chromatography is more suitable for the separation of alfacalcidol. Thin-layer chromatography has the advantages of large sample loading and short separation time, and its equipment is simple, easy to operate, and sample pretreatment is simple, but the separation The effect is poor, the error is large, the stereoisomers cannot be separated, and the recovery steps after separation are complicated, and the sample loss is large during the process

Medium-pressure liquid chromatography and high-performance liquid chromatography are commonly used in column chromatography. Medium-pressure liquid chromatography is relatively simple and has a large amount of sample loading; but its separation effect is poor, the chromatographic column can only be used once, and the column packing operation is complicated , the separation time is long, and it is difficult to solve the separation of complex mixtures

High-pressure liquid chromatography is suitable for organic compounds with high boiling point, non-...

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