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Production process of vitamin D2

A production process and vitamin technology, applied in the direction of organic chemistry, etc., can solve the problems of serious environmental pollution, low product purity, incomplete reaction, etc., and achieve the effect of simplifying process steps, improving process conditions, and facilitating process maintenance and process management

Active Publication Date: 2017-03-15
SICHUAN YUXIN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since ergosterol removes pre-vitamin D from photoreaction 2 In addition, it is very easy to generate toxic by-products photosterol, so this application adopts reagents such as pyridine and 3,5-dinitrobenzoyl chloride to separate and purify vitamin D through esterification and crystallization. 2 , the steps involved in the esterification crystallization method are numerous, and chemical reagents such as pyridine, 3,5-dinitrobenzoyl chloride or butyryl chloride need to be used for additional reactions, which seriously pollute the environment and cannot be completely reacted, and the purity of the obtained product is not high. high and low yield

Method used

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  • Production process of vitamin D2

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Add 10 kilograms of ergosterol and 300L methanol into the batching tank, start stirring and heat up to 32° C., and make a photoreaction solution with a concentration of 3 wt%, keep it warm for 1.5 hours, then pass the photoreaction solution through the flowmeter through the light source power of positive nitrogen gas. A 20kw ultraviolet irradiator is used for photochemical reaction, the temperature of the photoreaction solution is controlled at 50°C, the flow rate of the photoreaction solution is controlled at 120L / h, and then the irradiated reaction solution is concentrated under reduced pressure in a concentration pot, and the concentrate is transferred to Freeze and crystallize in a refrigerated stirring tank at -16°C for 10 hours, filter and recover unreacted raw materials, react the filtrate at 60°C and -0.08Mpa for 2 hours to obtain 1.5 kg of transformed oil, and detect vitamin D in the transformed oil by liquid phase 2 The content is 80wt%; 1.5 kg of converted oil...

Embodiment 2

[0029] Add 15kg of ergosterol, 350L of methanol and 280L of cyclohexane into the batching tank, start stirring and heat up to 30°C, make a photoreaction solution with a concentration of 2wt%, keep it warm for 2 hours, and then pass the photoreaction solution through the flowmeter through the positive channel. The light source power of nitrogen is 30kw ultraviolet irradiator for photochemical reaction, the temperature of the photoreaction solution is controlled at 40°C, the flow rate of the photoreaction solution is controlled at 110L / h, and then the irradiated reaction solution is concentrated under reduced pressure in a concentration pot. Transfer the concentrate to a refrigerated and stirred tank at -15°C for freezing and crystallization for 8 hours, filter and recover unreacted raw materials, and react the filtrate at 65°C and -0.09Mpa for 1.5 hours to obtain 1.8 kg of invert oil. Vitamin D 2 The content is 83wt%; the converted oil and 2 times the amount of ethyl acetate ar...

Embodiment 3

[0031] Add 12 kilograms of ergosterol and 260L ethanol into the batching tank, start stirring and heat up to 35° C., and make a photoreaction solution with a concentration of 4 wt %, keep it warm for 1 hour, and then pass the photoreaction solution through the flowmeter through the light source power of positive nitrogen gas. A 25kw ultraviolet irradiator is used for photochemical reaction, the temperature of the photoreaction solution is controlled at 60°C, the flow rate of the photoreaction solution is controlled at 130L / h, and then the irradiated reaction solution is concentrated under reduced pressure in a concentration pot, and the concentrate is transferred to Freeze and crystallize at -20°C for 5 hours in a refrigerated and stirred tank, filter and recover unreacted raw materials, react the filtrate at 70°C and -0.095Mpa for 1 hour to obtain 1.68 kg of transformed oil, and detect vitamin D in the transformed oil by liquid phase 2 The content is 83wt%; the converted oil a...

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Abstract

The invention discloses a production process of vitamin D2. The process includes the steps of: S1) light irradiation and thermal-isomerization reaction; S2) chromatographic eluting separation; S3) freezing crystallization separation; S4) drying, mixing and packaging. Compared with the prior art, the process is modified in synthetic process conditions, so that the process is improved in productivity and total yield of the product reaches more than 90%. The thermal-isomerization reaction and a pressure-reduced concentration step are combined, so that the process is simplified and is reduced in energy consumption. A synthesis reaction zone and a purifying separation zone are completely separated, so that process maintenance and process management are convenient. In addition, in the purifying process, a chromatographic crystallization method is employed directly instead of a process comprising chromatography, esterification and hydrolytic crystallization in the prior art, so that usage of toxic organic reagents is avoided, and the process is energy-saving, reduces consumption and is environment-friendly. In the production process of the vitamin D2, tail oil and tail materials contain lumisterol, tachysterol and other derivative products, so that it is valuable to deeply research and develop a high-value medicine intermediate.

Description

technical field [0001] The invention relates to the field of fine chemical industry, in particular to a kind of vitamin D conforming to the standard of Pharmacopoeia 2 production process. Background technique [0002] Vitamin D 2 (Vitamin D 2 ), the chemical name is 9,10-senoergosta-5,7,10(19),22-tetraen-3β-ol. It is colorless needle-like crystal or white crystalline powder; odorless and tasteless; easily deteriorated when exposed to light or air. For the prevention and treatment of vitamin D deficiency, chronic hypocalcemia, hypophosphatemia, rickets and osteomalacia with chronic renal insufficiency, familial hypophosphatemia and hypoparathyroidism (postoperative , idiopathic or pseudo hypoparathyroidism) treatment, for the treatment of acute, chronic and potential postoperative tetany and idiopathic tetany. [0003] Vitamin D 2 Promote the absorption of calcium by the brush border of the small intestinal mucosa and the reabsorption of phosphorus by the renal tubules,...

Claims

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Application Information

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IPC IPC(8): C07C401/00
CPCC07C401/00
Inventor 冷莉
Owner SICHUAN YUXIN PHARM CO LTD
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