Application background and overview of deuterated tetrahydrofuran
Tetrahydrofuran is a saturated cyclic ether composed of four carbon atoms. It is miscible with water and compatible with general organic solvents (ethanol, ether, aliphatic hydrocarbons, halogenated hydrocarbons, etc.) and is an excellent solvent. It is usually produced by dehydration of 1,4-butanediol or hydrogenation of furan. Long-term contact with air will cause auto-oxidation and generate explosive peroxides. Before being used as a solvent for chemical reactions, it must be pretreated to remove possible peroxides or antioxidants added to prevent auto-oxidation.
Before pretreatment distillation or heating, you should first check whether there is peroxide with 2% acidic potassium iodide solution, wash with a mixed aqueous solution of ferrous sulfate and sulfuric acid, or reflux with lithium aluminum hydride before distilling to remove water. , peroxides, antioxidants and other impurities. It is a flammable liquid with low boiling point and flash point. It is easy to catch fire at room temperature. It must be kept away from fire sources when used. It has an irritating effect on the skin and mucous membranes of the eyes, nose, and tongue. Its vapor is anesthetic. Inhaling high-concentration vapor for a long time can cause dizziness, dizziness, headache, vomiting, etc.
When its concentration in the blood reaches 160 mg%, it will cause complete anesthesia, and when it reaches 300 mg%, it can cause death. However, the pure product is less toxic than acetone and is one of the least toxic solvents. The maximum allowable concentration in the workplace is 200ppm, and its smell can be smelled when it is greater than 25-50ppm. There is no danger in general use. Should be stored in a cool, ventilated and dry place. Tetrahydrofuran-d8, whose English name is Tetrahydrofuran-d8, also known as deuterated tetrahydrofuran, and whose molecular formula is C4D8O, is a chemical intermediate.
Application structure of deuterated tetrahydrofuran
Applications of deuterated tetrahydrofuran
Tetrahydrofuran serves as an excellent solvent in Grignard reactions, polymerization reactions, reduction reactions with lithium aluminum hydride, condensed fluorophenylboronic acid reactions and esterification reactions. It has a fast dissolution speed and good penetration and diffusion properties on the surface and interior of the resin, so it is widely used. Use it to dissolve polyvinyl chloride, polyvinylidene chloride and other copolymers to obtain a low-viscosity solution, which can be used in the manufacture of surface protective coatings, adhesives and films. It can also be used for the preparation of inks and paint stripping. Agents, extraction agents and artificial leather surface treatment agents, etc. In the presence of zinc chloride, it reacts with acid or acid chloride to easily open the ring and generate 1,4-butanediol and 1,4-dichlorobutane. Heating with hydrogen chloride gas can produce 4-chloro-1-butanol.
Tetrahydrofuran can also be used as a raw material for the synthesis of butadiene, nylon, polybutylene glycol ether, γ-butyrolactone, polyvinylpyrrolidone, tetrahydrothiophene, etc. Deuterated tetrahydrofuran is mainly used as a pharmaceutical intermediate. Examples of its applications are as follows:
Deuterated tetrahydrofuran is used as a solvent to prepare semiconductor catalysts. Including the following raw materials: cadmium selenide or cadmium sulfide quantum dots, and salts or complexes of cobalt, nickel or iron. The present invention is a method for preparing a high-efficiency semiconductor catalyst from cadmium selenide or cadmium sulfide quantum dots through a photochemical method and photolyzing water to produce hydrogen in the presence of an electron sacrificial body. It can be easily and quickly realized to be driven by visible light from cadmium selenide or cadmium sulfide quantum dots. A high-efficiency semiconductor catalyst, aminoguanidine bicarbonate, was prepared in situ by photoreaction and photolyzed water to produce hydrogen in the presence of an electron sacrificial body. The hydrogen production rates can reach 40 μmol·h-1·mg-1 (CdSe) and 25 μmol·h-1·mg-1 (CdS) respectively.
The preparation method includes the following specific steps:
1) In a transparent reactor, add water-soluble cadmium selenide or cadmium sulfide quantum dots;
2) Add the water or organic solution of the electron sacrificial body to the reactor to obtain mixed solution A;
3) Add a salt or complex solution of cobalt, nickel or iron to the mixed liquid A obtained in step 2) to obtain a mixed liquid B;
4) Add water or a mixed solvent of water and a water-miscible organic solvent to the mixed liquid B obtained in step 3) to obtain a mixed liquid C; in the mixed solvent of water and a water-miscible organic solvent, The organic solvent is acetonitrile, tetrahydrofuran, dimethylformamide, methanol, ethanol, propanol, acetone, deuterated water, deuterated acetonitrile, deuterated tetrahydrofuran, deuterated dimethylformamide, deuterated methanol, deuterated Ethanol, deuterated propanol or deuterated acetone. Preferably, the volume ratio of water:organic solvent=1:0.5~5;
5) Add an appropriate amount of acid solution or alkali solution to the mixed liquid C obtained in step 4), and adjust the pH value so that the pH of the system=4~11; to obtain mixed liquid D;
6) Pour inert gas into the reactor filled with mixed liquid D, or evacuate the transparent reactor filled with mixed liquid D; in an inert gas or vacuum atmosphere, use wavelength = nm ~ 780nm Visible light irradiates the reactor. After the reaction is completed, the centrifuge precipitates to obtain a semiconductor catalyst for the photocatalytic hydrogen production system.
