3,3-Dialkylthio-2-phenylselenyl-2-propene-1-one derivatives and their synthesis
A technology of dialkylthio and phenylselenyl, which is applied in the field of 3,3-dialkylthio-2-phenylselenyl-2-propene-1-one derivatives and synthesis, which can solve the problem of complex operation and low yield Low-cost problems, to achieve the effect of high product yield, simple steps, cheap and easy-to-obtain raw materials
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Embodiment 1
[0026]
[0027] In a 25mL reaction tube, add p-TsOH·H 2 O (2.9 mg, 0.015 mmol), 3,3-dialkylthio-2-propen-1-one 2a (48.7 mg, 0.30 mmol), organoselenium reagent 3a (99.7 mg, 0.33 mmol) and 3 mL of solvent 1, 2-Dichloroethane, reacted at 30°C for 5h. After the reaction, the volatile components were removed under reduced pressure, and then separated by silica gel column chromatography (eluent was petroleum ether (60-90°C / dichloromethane, v / v=2:1) to obtain the light yellow solid target Product 1a (91.4 mg, yield 96%). The target product was confirmed by NMR and high-resolution mass spectrometry.
Embodiment 2
[0029]
[0030] The reaction steps and operations are the same as in Example 1, except that the organic selenium reagent is 3b phenylselenyl chloride (63.2 mg, 0.33 mmol). The reaction was stopped, and the target product 1a (47.6 mg, yield 50%) was obtained after post-processing. It shows that the effect of organic selenium reagent 3b is not as good as that of organic selenium reagent 3a.
Embodiment 3
[0032] The reaction steps and operations are the same as in Example 1, except that the reaction temperature is 0°C. The reaction was stopped, and the target product 1a (87.6 mg, yield 92%) was obtained after post-processing.
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