Vitamin D3 purification method

A purification method and vitamin technology, applied in the direction of organic chemistry and the like, can solve the problems of unfavorable packaging, storage and transportation process, reduce the stability of vitamin D, etc., and achieve the effects of not easy to degrade, not easy to decompose, and high product yield.

Active Publication Date: 2021-03-12
弘健制药(上海)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The inventor believes that the purity of vitamin D3 purified by the current purification method needs to be improved, and because the purified vitamin D3, these harmful impurities will promote the degradation of vitamin D3 under high temperature, high humidity and strong light conditions, and reduce the vitamin D3 is not conducive to the later packaging, storage and transportation process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] a form of vitamin D 3 The purification method comprises the following steps:

[0048] a. Esterification reaction

[0049] a1. Mix and stir 15.8kg triethylamine and 104kg dichloromethane in the reaction kettle first, then add 8kg vitamin D 3 Oil, control the internal temperature of the reactor below 25°C, slowly add 7.2kg of benzoyl chloride into the reactor, then adjust the internal temperature at 30°C, keep the temperature for 2.5h, then add 16kg of pure water into the reactor, and stir for 7.5min , let stand for 12.5min, terminate the reaction, and transfer the lower organic phase;

[0050] a2. Wash the organic phase three times with 48kg of pure water, then add 8kg of anhydrous sodium sulfate to stir and dehydrate for 30 minutes, then filter with 4kg of neutral alumina, control the internal temperature below 35°C, and the vacuum degree below -0.06MPa. Add 96kg of acetone after pressure distillation to near dryness, raise the temperature to 45°C, stir and dissolve ...

Embodiment 2

[0058] a form of vitamin D 3 The purification method comprises the following steps:

[0059] a. Esterification reaction

[0060] a1. Mix and stir 15.76kg of pyridine and 100kg of methanol in the reactor first, then add 8kg of vitamin D 3 Oil, control the internal temperature of the reactor below 25°C, slowly add 6.8kg of 3,5-dinitrobenzoyl chloride into the reactor, then adjust the internal temperature at 25°C, keep the temperature for 2 hours, and then add 14.4kg of pure water to In the reaction kettle, stir for 5 minutes, let stand for 10 minutes, terminate the reaction, and transfer the lower organic phase;

[0061] a2. Wash the organic phase three times with 48kg of pure water, then add 8kg of anhydrous sodium sulfate, stir and dehydrate for 35min, then filter with 4kg of neutral alumina, control the internal temperature below 35°C, and reduce the vacuum degree below -0.06MPa. Add 92kg of acetone after pressure distillation to near dryness, raise the temperature to 40°C...

Embodiment 3

[0069] a form of vitamin D 3 The purification method comprises the following steps:

[0070] a. Esterification reaction

[0071] a1. First mix 15.84kg triethylamine and 108kg ethanol in the reaction kettle, then add 8kg vitamin D 3 Oil, control the internal temperature of the reactor below 25°C, slowly add 7.6kg of benzoyl chloride into the reactor, then adjust the internal temperature at 35°C, keep the temperature for 3 hours, then add 17.6kg of pure water into the reactor, stir for 10min, Stand still for 15min, terminate the reaction, transfer the lower organic phase;

[0072] a2. Wash the organic phase three times with 48kg of pure water, then add 8kg of anhydrous sodium sulfate, stir, dehydrate and dry for 40min, then filter with 4kg of neutral alumina, control the internal temperature below 35°C, and reduce the vacuum degree below -0.06MPa. Add 100kg of acetone after pressure distillation to near dryness, raise the temperature to 50°C, stir and dissolve for 30 minutes, t...

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PUM

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Abstract

The invention discloses a vitamin D3 purification method which comprises the following steps: a1, mixing organic amine, a first organic solvent, vitamin D3 oil and aryl chloride to react, and then adding water to stop the reaction; a2, washing the product obtained in the step a1 with water, performing drying and filtering, carrying out reduced pressure distillation, performing dissolving, carryingout secondary reduced pressure distillation, carrying out cooling and crystallizing; b1, dissolving vitamin D3 methyl benzoate in methanol, and dropwise adding a strong alkaline solution to perform reacting; b2, carrying out reduced pressure distillation on the substance obtained in the step b1, then carrying out liquid separation, washing an organic phase with water, and carrying out drying, filtering, carrying out secondary reduced pressure distillation, dissolving, cooling and recrystallizing; c1, dissolving the vitamin D3 crude product in a third organic solvent, and then performing stirring for decolorization; and c2, filtering the product obtained in the step c1, carrying out reduced pressure distillation on the filtrate, and carrying out dissolving, cooling, recrystallizing, filtering, and drying to obtain the vitamin D3. The vitamin D3 purified by the purification method disclosed by the invention has the advantages of higher purity, lower harmful impurity content and higher stability.

Description

technical field [0001] This application relates to the field of fine chemicals, more specifically, it relates to a vitamin D 3 purification method. Background technique [0002] Vitamin D 3 Also known as cholecalciferol, it is a kind of vitamin D. It can only be dissolved in fat or fat solvent. It can withstand high temperature and oxidation in neutral and alkaline solutions. It can improve the body's absorption of calcium and phosphorus, and make plasma calcium and plasma phosphorus levels reach saturation levels. With the international vitamin D 3 Plenty of In-Depth Research, Vitamin D 3 It is widely used to make potions to treat various diseases. [0003] Vitamin D 3 The production method is usually to dissolve 7-dehydrocholesterol in ethanol, then irradiate the ring with ultraviolet light, concentrate the reaction solution, freeze and filter, and then pass nitrogen gas into the filtrate and concentrate it to dryness under reduced pressure to obtain vitamin D 3 Oil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C401/00
CPCC07C401/00C07C2601/14C07C2602/08
Inventor 汪武训戚兴凯孙春亮高岩松周秋火柏挺华吉涛
Owner 弘健制药(上海)有限公司
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