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Method for producing selenol

A manufacturing method and technology for selenol, applied in directions such as organic chemistry, can solve the problems of variable yield, unpredictable yield of selenols, low yield of selenols, etc., to suppress the deviation of yield, practical High-performance, high-yield effect

Inactive Publication Date: 2015-04-15
SUMITOMO SEIKA CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, in the method of Non-Patent Document 1, there is a shortcoming that the yield of selenols is low
Moreover, in the method of Non-Patent Document 1, since the yield of each batch of preparation varies, the yield of the finally obtained selenols cannot be predicted in advance, and there are also problems in the commercial production of selenols.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

manufacture example 1

[0083] 194.5 g (8.00 mol) of magnesium and 601.6 g of diethyl ether were added to a 3 L four-necked flask equipped with a stirrer, a thermometer, and a reflux cooling tube. A p-bromotoluene solution in which 1368.2 g (8.00 mol) of p-bromotoluene was dissolved in 600.0 g of diethyl ether was prepared, and 1 / 10 of the solution was added to the above-mentioned four-necked flask. The reaction liquid was heated to 40° C. using an oil bath to initiate the Grignard reaction. Then, after adding the remaining p-bromotoluene solution dropwise, reaction was performed for 1 hour to obtain 2764.4 g of p-tolyl magnesium bromide solution (purity: 1547.1 g, 7.92 mol).

Embodiment 1

[0085] In a four-neck flask with a capacity of 500 mL having a stirrer, a thermometer and a reflux cooling tube, 174.5 g (purity 97.6 g, 0.50 mol) of the p-tolyl magnesium bromide solution obtained in Production Example 1 was added, and the reaction solution was cooled to 0° C. Thereafter, while maintaining the range of 0 to 10°C, 47.4 g (0.50 mol) of selenium powder was added to obtain a reaction liquid containing a selenium magnesium halide. In a four-necked flask with a 500mL capacity of a stirrer, a thermometer and a reflux cooling tube, add a mixed solution (pH value of less than 1) of 35% by mass hydrochloric acid 83.3g (0.80mol) and pure water 200.8g, and the obtained reaction solution After the total amount of the solution was added dropwise so as not to exceed the range of 0 to 30° C., the mixture was incubated with continuous stirring for about 1 hour, and the organic layer was collected.

[0086] The recovered organic layer was analyzed by the absolute calibration c...

Embodiment 2

[0088] As a result of producing p-tolylselenol four times under the same conditions as in Example 1, the yields were 85.7%, 86.3%, 85.3%, and 85.8% for the Grignard reagent. That is, from the present results, it was confirmed that p-tolylselenol can be stably produced with a high yield without variation in the yield by batch production according to the production method of the present invention.

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PUM

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Abstract

The main purpose of the present invention is to provide a method for producing a selenol with high yield without causing the fluctuations in yield among production lots. The purpose can be achieved by a method for producing a selenol, which comprises steps (1) and (2): (1) a step of reacting a Grignard reagent represented by general formula (1) with selenium to produce a reaction solution containing a selenomagnesium halide represented by general formula (2); and (2) a step of adding the reaction solution produced in step (1) mentioned above to an acidic solution dropwisely to produce a selenol represented by general formula (3).

Description

technical field [0001] The present invention relates to a method capable of producing selenols with a high yield and with little variation in the yield produced between batches. Background technique [0002] Selenols are essential compounds in the field of electronic materials and medicine-related fields, and many studies have been conducted on their physical properties and utilization methods. There are many methods for synthesizing selenols, and a generally known method is to synthesize them by reacting a Grignard reagent with selenium and then protonating them. For example, in Non-Patent Document 1, the method for synthesizing phenylselenol is disclosed. After the reaction of magnesium chips and bromobenzene in anhydrous ether to prepare the Grignard reagent, the selenium powder is slowly added to maintain a slow reflux state to prepare A reaction solution containing a selenomagnesium halide. Furthermore, it discloses the method of pouring the obtained reaction liquid i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C391/02
CPCC07C391/02
Inventor 高野胜己白石浩之坂上茂树
Owner SUMITOMO SEIKA CHEM CO LTD
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