A nitrogen-containing heterocyclic nitrogen oxide derivative and its preparation method
A technology of nitrogen oxides and nitrogen heterocycles, which is applied in the field of nitrogen-containing heterocycle nitrogen oxide derivatives and its preparation, can solve the problems of few types and limited applications, and achieve the advantages of convenient operation, simple process and wide application range Effect
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Embodiment 1
[0035] The nitrogen-containing heterocyclic nitrogen oxide derivative of this embodiment is 2-phenylthioquinoline nitrogen oxide, and its structural formula is:
[0036]
[0037] The preparation method of the nitrogen-containing heterocyclic nitrogen oxide derivative of the present embodiment, the reaction scheme is as follows:
[0038]
[0039] Specifically take the following steps:
[0040] 1) Take 0.25mmol of quinoline nitrogen oxide, 0.45mol of diphenyl disulfide, Cu(AcO) 2 Add 0.125 mmol and 0.5 mmol of potassium hydroxide to 1 mL of toluene to prepare a mixture, place the mixture in a 5 mL Schlenk tube, heat it in an oil bath at 130°C, react for 48 hours, and cool to room temperature to obtain a reaction solution;
[0041] 2) The reaction solution was concentrated to obtain a concentrate, and the concentrate was separated by thin-layer chromatography using a mixed solvent composed of ethyl acetate and petroleum ether in a volume ratio of 1:2 as a developing solve...
Embodiment 2
[0044] The nitrogen-containing heterocyclic nitrogen oxide derivative of the present embodiment is 2-(4-methylphenylthio)quinoline nitrogen oxide, and its structural formula is:
[0045]
[0046]The preparation route of the nitrogen-containing heterocyclic nitrogen oxide derivatives of this embodiment can refer to Example 1, and the following steps are specifically adopted:
[0047] 1) Take 0.25mmol of quinoline nitrogen oxide, 0.45mmol of p-toluene disulfide, Cu(AcO) 2 Add 0.125 mmol and 0.5 mmol of potassium hydroxide to 1 mL of toluene to prepare a mixture, place the mixture in a 5 mL Schlenk tube, heat it in an oil bath at 130°C, react for 48 hours, and cool to room temperature to obtain a reaction solution;
[0048] 2) The reaction solution was concentrated to obtain a concentrate, and the concentrate was separated by thin-layer chromatography using a mixed solvent composed of ethyl acetate and petroleum ether in a volume ratio of 1:2 as a developing solvent and silica...
Embodiment 3
[0051] The nitrogen-containing heterocyclic nitrogen oxide derivative of this embodiment is 2-benzylthioquinoline nitrogen oxide, and its structural formula is:
[0052]
[0053] For the nitrogen-containing heterocyclic nitrogen oxide derivatives of this embodiment, the reaction scheme can refer to Example 1, and the following steps are specifically adopted:
[0054] 1) Take quinoline nitrogen oxide 0.25mmol, dibenzyl disulfide 0.45mmol, Cu(AcO) 2 0.125mmol and 0.5mmol of potassium hydroxide were added to 1mL of toluene to prepare a mixture, the mixture was placed in a 5ml Schlenk tube, heated in an oil bath at 130°C, and reacted for 48h, then cooled to room temperature to obtain a reaction solution;
[0055] 2) The reaction solution was concentrated to obtain a concentrate, and the concentrate was separated by thin-layer chromatography using a mixed solvent composed of ethyl acetate and petroleum ether in a volume ratio of 1:2 as a developing solvent and silica gel as an a...
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