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Method and device for preparing calcitriol by utilizing photochemical reaction

A technology of photochemical reaction and calcitriol, which is applied in chemical industry, organic chemistry, chemical/physical/physicochemical process of energy application, etc., can solve undiscovered problems and achieve convenient operation, energy saving and strong environmental protection Effect

Active Publication Date: 2009-12-23
CP PHARMA QINGDAO CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Taking a comprehensive view of the above-mentioned documents and patented technologies, no effective method and technical device have been found to directly convert the 5,6-trans isomer, which is discarded in the existing calcitriol production process, into calcitriol

Method used

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  • Method and device for preparing calcitriol by utilizing photochemical reaction
  • Method and device for preparing calcitriol by utilizing photochemical reaction
  • Method and device for preparing calcitriol by utilizing photochemical reaction

Examples

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Effect test

Embodiment 1

[0021] This embodiment is carried out in a reaction device, 1 g of a 5,6-trans isomer sample with a purity greater than 95% is dissolved in 1000 ml of absolute ethanol; the selected light reaction temperature is 25 ± 5 ° C, and the circulation flow rate is 50 ml / min, after the photochemical reaction is completed, the reaction solution is concentrated to dryness with a rotary evaporator to obtain a light yellow solid, which is recrystallized with ethyl acetate-n-pentane at a volume ratio of 1:3 to obtain white needle crystals 0.732g; detected by HPLC, the content is 99.6%, by IR, UV-VIS, 1 HNMR, 13 CNMR and other spectra confirmed that the product obtained by the photochemical reaction was calcitriol, and the conversion rate of the light reaction was 76.9%.

Embodiment 2

[0023] This example is carried out in a reaction device, 1 g of a sample with a 5,6-trans isomer purity greater than or equal to 95% is dissolved in 5000 ml of absolute ethanol; the light reaction temperature is adjusted to 25 ± 5 ° C, and the circulation flow rate is 50 ml / min, after the photochemical reaction is completed, the reaction solution is concentrated to dryness with a rotary evaporator under reduced pressure to obtain a light yellow solid and ethyl acetate-n-pentane at a volume ratio of 1:3 for recrystallization to obtain 0.758 g of white needle crystals ; Detected by HPLC, the content is 99.8%, by IR, UV-VIS, 1 HNMR, 13 CNMR and other spectra confirmed that the product obtained by the photochemical reaction was calcitriol, and its photoreaction conversion rate was 78.5%.

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Abstract

The invention relates to a method and a device for preparing calcitriol by utilizing photochemical reaction. 5,6- trans isomer aborted as impurity in the existing production process of the calcitriol is converted into the calcitriol through the photochemical reaction, thereby the production yield of the calcitriol is increased by 50 percent, and the method for preparing the calcitriol by utilizing the photochemical reaction is carried out in a reaction device. The major structure comprises a reactor containing a clamping sleeve, a quartz glass light tube low-pressure mercury light and a low-temperature cooling liquid recycle pump, wherein the reactor is internally provided with the clamping sleeve, an inner sleeve adopts heat-resistant quartz glass, and an outer sleeve adopts the heat-resistant quartz glass the outer wall of which is plated with silver mirror; the mercury light is arranged in the inner sleeve of the reactor; reaction liquid is arranged in the outer sleeve of the reactor; and the outer sleeve of the reactor is provided with an upper outlet and a lower outlet. The preparation method has simple technical process, easy control of reaction, high product yield and strong environmental protection, and the device has simple structure, convenient operation, energy saving and good product yield.

Description

Technical field: [0001] The invention relates to a method and device for preparing calcitriol by photochemical reaction. The 5,6-trans isomer discarded as impurities in the existing production process of calcitriol is converted into Calcitriol, thereby increasing the production yield of calcitriol by about 50%. Background technique: [0002] Calcitriol is Vitamin D 3 It is a substance that finally works after being metabolized by 25-hydroxylase in the liver and 1α-hydroxylase in the kidney. It is currently clinically used to treat osteoporosis, hypoparathyroidism, and renal osteodystrophy. . Calcitriol has a variety of synthetic routes, which are currently used in the literature (HerbertE.Paaren, Hector F.Deluca, and Heinrich K.Schnoes; Direct C(1) Hydroxylation of vitaminD3and Related Compounds, J.org.chem.1980 , 45, 3253-3258) synthetic route, the advantage of this synthetic route is that there are few synthetic steps and short production cycle, and the chemical reagent...

Claims

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Application Information

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IPC IPC(8): C07C401/00B01J19/12
CPCY02P20/10
Inventor 王明刚任莉陈阳生孙桂玉
Owner CP PHARMA QINGDAO CO LTD
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