Photosensitized oxidation reaction equipment and application thereof

A technology of photosensitive oxidation and reaction equipment, applied in the chemical/physical/physical-chemical process of applying energy, etc., can solve the problems of reaction dead zone, low degree of turbulence, small height and diameter, etc., and achieve high utilization of light and photoelectric conversion. The effect of high rate and reduced complexity

Active Publication Date: 2014-05-14
HUNAN KEYUAN BIO PRODS
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The built-in photoreactor mainly has the following problems: 1) The height and diameter of the traditional reactor photoreactor are relatively small, and the gas-liquid mixing is uneven, especially near the wall of the reactor, which is easy to form a reaction dead zone; 2) The traditional reactor The internal liquid mixing in the tank-type photoreactor is forced to circulate by the external pump, the degree of turbulence in the tank is low, and uniform reaction cannot be guaranteed; 3) There is no safe heat removal method in the traditional tank-type photoreactor, which has a large safety hazard
Because of these factors, photooxidative reactions have placed some limitations on large-scale production in organic chemistry.

Method used

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  • Photosensitized oxidation reaction equipment and application thereof
  • Photosensitized oxidation reaction equipment and application thereof
  • Photosensitized oxidation reaction equipment and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Dissolve 10 Kg of citronellol in 50L of dichloromethane, add 10g of tetraphenylporphyrin therein, and stir evenly; divide into 10 parts, add in 10 photoreactors 2 respectively, and place the constant temperature tank 1 The temperature drops to -30 o C, after half an hour of passing oxygen through the interface 2-6 at the bottom of the chromatography column 2-1, turn on the LED light source, and allow the reaction system to remain at this temperature for 10 hours; then, slowly return the temperature of the thermostat 1 to At room temperature (25°C), collect the reaction solution, add 100Kg of saturated sodium thiosulfate solution, stir thoroughly for 1 hour, and separate the liquids; then add 30Kg of saturated sodium thiosulfate solution to the dichloromethane phase, stir well, and separate the organic phase; dry the organic phase with anhydrous sodium sulfate; filter, separate the aqueous phase from the dichloromethane phase, add 50 g of concentrated sulfuric acid to th...

Embodiment 2

[0045] Dissolve 10Kg of dihydroartemisinic acid in 60L of toluene, add 5g of photosensitizer tetraphenylporphyrin and 2Kg of trifluoroacetic acid into the system, stir, divide into 10 parts, and add to 10 photoreactors 2 respectively , lower the temperature of the constant temperature tank 1 to -40°C, slowly introduce air from the interface 2-6 at the bottom of the chromatography column 2-1 for half an hour, turn on the LED light source, and let the reaction system react at this temperature for 5 hours; then , the temperature of the thermostat 1 was slowly returned to room temperature (25° C.), and the reaction was carried out for 1 hour. Turn off the light source, stop feeding the air, pour out the reaction solution, add saturated NaHCO 3 20 L of aqueous solution was stirred, the organic phase was separated, the organic phase was dried, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain crude artemisinin, which was...

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Abstract

The invention relates to photosensitized oxidation reaction equipment and application of the photosensitized oxidation reaction equipment. The photosensitized oxidation reaction equipment consists of a thermostatic bath and more than three photoreactors, wherein the photoreactors are fixed in the thermostatic bath and comprise a chromatographic column with a sand core; the middle of the chromatographic column is inlayed with a glass tube; a reaction system cavity is arranged between the chromatographic column and the glass tube; a light source is arranged in the middle of the glass tube; and an interface with a piston is arranged at the bottom of the chromatographic column. The equipment is used for photosensitized oxidization reaction, the photosensitizer is preferably tetraphenylporphyrin or a tetraphenylporphyrin derivative, the integrating degree between the absorption spectrogram of the tetraphenylporphyrin or the derivative thereof and the spectrogram of an LED light source is high, so that the light utilization ratio is high and the use amount of the photosensitizer is low. The photosensitized oxidation reaction equipment is simple in structure, low in manufacturing cost and safe and convenient to operate.

Description

technical field [0001] The invention relates to a photosensitive oxidation reaction device and its application, in particular to a large-scale photosensitive oxidation reaction device and its application. Background technique [0002] Photosensitive oxidation reaction is one of the photochemical reactions with important practical significance in organic synthesis, especially in the synthesis of medicinal spices and the like. For example, prostaglandins, which have important uses in family planning and disease treatment, are difficult to prepare by biochemical or other methods. And through the photooxidation reaction, the prostaglandin PGE with physiological activity can be obtained from arachidonic acid in only two steps. 2 (See Xiao Xuling et al., Science of China, 24(5), 648(1981)). In terms of anti-tumor active drugs, Costedo et al. have reported the total synthesis of Pontevedrine (Scheme 1) using the [4+2] addition reaction of singlet oxygen and double bonds (see Cost...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/12
Inventor 林文彬刘志强
Owner HUNAN KEYUAN BIO PRODS
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