A kind of preparation method of nitrooleic acid and its derivatives
A technology of nitrooleic acid and its derivatives, which is applied in the preparation of nitrooleic acid or nitrooleic acid methyl ester, and in the field of preparation of nitrooleic acid and its derivatives. It can solve problems such as complex methods and achieve synthesis steps simple effect
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Embodiment 1
[0032] Weigh 0.592 g (0.002 mol) of the purified methyl oleate, dissolve it in 20 ml of n-hexane dewatered by molecular sieves, and obtain a methyl oleate solution. Prepare 160ml of sulfuric acid aqueous solution with a concentration of 3wt%, weigh 2.76g (0.04mol) NaNO 2 Dissolve in 20ml of deionized water, add 5ml dropwise to the sulfuric acid aqueous solution with a dropping funnel every 30min, add dropwise 4 times, stir rapidly at room temperature, and remove the generated gas (NO 2 ) into the methyl oleate solution at a flow rate of 2.5ml / min, and after continuous nitration reaction for 4 hours, nitrogen gas was continuously introduced for 30 minutes to remove NO in the solution 2 gas. The reaction product was distilled under reduced pressure, dissolved in chloroform, and separated by thin layer chromatography (Merck's silica gel preparation plate PLCSilicagel60F254, the developing solvent was n-hexane:chloroform:ethyl acetate=60:13:4) to obtain nitro oil Acid methyl est...
Embodiment 2
[0037] Weigh 0.564 g (0.002 mol) of purified oleic acid and dissolve it in 20 ml of n-hexane dewatered by molecular sieves to obtain an oleic acid solution. Prepare 160ml of sulfuric acid aqueous solution with a concentration of 3wt%, weigh 2.76g (0.04mol) NaNO 2 Dissolve in 20ml of deionized water, add 5ml dropwise to the sulfuric acid aqueous solution with a dropping funnel every 30min, add dropwise 4 times, stir rapidly at room temperature, and remove the generated gas (NO 2 ) into the oleic acid solution at a flow rate of 2.5ml / min. After continuous nitration reaction for 4 hours, nitrogen gas was continuously passed for 30 minutes to remove NO in the solution. 2 gas. The reaction product was distilled under reduced pressure, dissolved in chloroform, and separated by thin-layer chromatography (Merck's silica gel preparation plate PLCSilicagel60F254, the developing solvent was n-hexane:ethyl acetate:acetic acid=60:4:3) to obtain nitro oil The acid product is 0.078g with a...
Embodiment 3
[0040] All the reaction raw materials and operating methods used are the same as in Example 1, except that the nitration reaction time is 12 hours, and the nitromethyl oleate product is prepared.
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