A kind of method of synthesizing diselenide

A technology of diselenide and selenium powder, applied in organic chemistry and other directions, can solve the problems of not conforming to the spirit of green chemistry, harsh reaction conditions, and difficulty in large-scale production, and achieve simple reaction, low equipment corrosion, and low cost. Effect

Active Publication Date: 2016-09-21
四川硒莱坞科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, from the current literature reports, usually diselenide is prepared by the reaction of selenium and Grignard reagent or sodium diselenide with halogenated hydrocarbons and sulfonic acid esters. These methods have long routes and harsh conditions for some reactions, resulting in The odorous intermediate selenol does not conform to the spirit of green chemistry, which makes the reaction cost high and pollutes the environment, making it difficult to apply to large-scale production

Method used

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  • A kind of method of synthesizing diselenide
  • A kind of method of synthesizing diselenide
  • A kind of method of synthesizing diselenide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Step 1: Add 252 mg (2 mmol) of anhydrous sodium sulfite and 158 mg (2 mmol) of selenium powder into the high-pressure sealed tube, vacuumize and fill with nitrogen, then add 2 ml of water into the high-pressure sealed tube, and then vacuumize Then fill it with nitrogen, then place it in an oil bath at 100°C and stir for 10 hours to react to obtain sodium selenosulfate.

[0020] Step 2: Mix 137 mg (1 mmol) of n-bromobutane, 1 ml of ethanol and the whole amount of sodium selenosulfate prepared above in another high-pressure sealed tube, and stir in an oil bath at 140°C for 10 hours. After the reaction, it was extracted with ether and separated by climbing a board to obtain the product—diselenide, with a yield of 74.2%.

[0021] The above purification method can also adopt column chromatography or thin layer chromatography.

Embodiment 2

[0023] Other conditions are the same as embodiment 1, check the impact of different temperatures on the reaction in step 1), and the experimental results are shown in the table below:

[0024]

[0025] It can be seen from the above table that the yield is higher when the reaction temperature is 140° C. (Example 1).

Embodiment 3

[0027] Other conditions are the same as embodiment 1, check step 2) in different reaction temperatures, investigate the change result of final yield, as shown in the table below:

[0028]

[0029] It can be seen from the above table that the yield is the highest when the reaction temperature is 100°C (Example 1).

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Abstract

A diselenide synthesizing method relates to the technical field of chemical synthesis. The method employs selenium powder as a selenylation reagent and anhydrous sodium sulfite as an additive, so that the method has many advantages. The method is free of any metal reagents. Because that selenium is a necessary microelement of living bodies and is metabolizable in human body, the method is ecological-friendly. In addition, the method is carried out under a neutral environment, so that the method is less in corrosion on devices and a reaction system is durable. The method does not generate a selenol intermediate which has stink smell, so that the method is suitable for industrial production, is low in cost and short in route, is mild in reaction conditions and is simple in reaction operations.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to the synthesis technology of diselenide. Background technique [0002] The development of organic selenium chemistry is quite rapid, and the synthesis and new methods of many useful selenium reagents in organic synthesis have been discovered and reported continuously. [0003] Among them, diselenide is the most widely used selenium reagent in organic synthesis, and it can be transformed into a variety of useful organoselenium compounds, so it is the most widely used in organoselenium compounds. However, from the current literature reports, usually diselenide is prepared by the reaction of selenium and Grignard reagent or sodium diselenide with halogenated hydrocarbons and sulfonic acid esters. These methods have long routes and harsh conditions for some reactions, resulting in The foul-smelling intermediate selenol does not conform to the spirit of green chemistry, whi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C391/00
Inventor 俞磊凌海刘名轩刘永红
Owner 四川硒莱坞科技有限公司
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