Synthesis method for o-alkoxy selenide
A synthetic method, the technology of o-alkoxyl, which is applied in the field of pharmaceutical production and the preparation of organic reagents - o-alkoxy selenides, can solve the problems of unfavorable industrial production, corrosion of reaction equipment, and large use, and achieve eco-friendliness, Equipment less corrosive effect
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Embodiment 1
[0013] Embodiment 1, reaction formula is as follows:
[0014]
[0015] In a 25 ml round bottom flask, add 0.156 g of diphenyldiselenide (1 mmol) and 0.025 g of iodine (10 mol%), 0.104 g of styrene (1 mmol) and 0.057 g of hydrogen peroxide ( 0.5 mmol) was dissolved in 1 ml of ethanol, and the mixed solution was added into a round bottom flask and air was introduced into the reaction system. Illuminated by 200W incandescent light at room temperature, the reaction solution gradually turned reddish brown. The reaction was monitored by thin layer chromatography (developer: petroleum ether / ethyl acetate 30:1). The reaction was completed after 20 h, and the reaction solution was separated by column chromatography to obtain 0.304 g of a light yellow oily substance—o-alkoxyselenide, with a yield of 99%.
Embodiment 2
[0017] Other conditions are the same as embodiment 1, and different amounts of iodine are tested as catalysts, and the experimental results are shown in Table 1.
[0018] Table 1 Test of catalyst iodine dosage effect, light source 200w incandescent lamp:
[0019]
[0020] As can be seen from the above table, 10mol% iodine catalyst consumption, productive rate is the highest.
Embodiment 3
[0022] Other conditions are the same as in Example 1, and different amounts of hydrogen peroxide are tested, and the experimental results are shown in Table 2.
[0023] The inspection of table 2 oxidant dosage effect:
[0024]
[0025] It can be seen from the above table that the dosage of 50mol% hydrogen peroxide is the best.
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