Preparation method of alkylsalicylic acid and/or alkylsalicylate
A technology of alkyl salicylate and alkyl salicylic acid, applied in the field of alkyl salicylate and alkyl salicylic acid, can solve the problems of harsh reaction conditions and high processing cost, and achieve relatively mild reaction conditions , high conversion rate, easy to recycle
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preparation Embodiment 1
[0036] Synthesis of IL-1 as catalyst of 1-methyl-3-butylimidazole boron tetrafluoride salt-metaphosphoric acid-sodium dodecylbenzenesulfonate
[0037] Add 1mol N-methylimidazole and 1.05mol 1-bromobutane into a three-necked flask, 2 After purging for 20mim, start stirring and heat to 85°C for 30-36h. After the reaction was completed, it was left to cool down to room temperature, the lower layer of the solution was light yellow, and the upper layer was unreacted raw materials. The upper layer liquid was decanted, 3 times the volume of ethyl acetate was added to the lower layer liquid to wash, and then the ethyl acetate was separated to remove unreacted raw materials. After washing, dry at 70°C for 24 hours to obtain light yellow viscous 1-methyl-3-butylimidazolium bromide.
[0038] The obtained 1-methyl-3-butylimidazolium bromide was dissolved in dichloromethane, and NaBF was added thereto 4 Aqueous solution with a content of 1mol was stirred and reacted at room temperature ...
preparation Embodiment 2
[0041]Synthesis of IL-2 Catalyst of 1-Methyl-3-Butylimidazolium Sulfate-Tripolyphosphoric Acid-Sodium Caprate
[0042] In the three-necked flask, add 1mol N-methylimidazole, 1.05mol 1-bromo-n-butane, pass through N 2 After purging for 20mim, start stirring and heat to 85°C for 30-36h. After the reaction was completed, it was left to cool down to room temperature, the lower layer of the solution was light yellow, and the upper layer was unreacted raw materials. The upper layer liquid was decanted, 3 times the volume of ethyl acetate was added to the lower layer liquid to wash, and then the ethyl acetate was separated to remove unreacted raw materials. After washing, dry at 70°C for 24 hours to obtain light yellow viscous 1-methyl-3-butylimidazolium bromide.
[0043] Dissolve the obtained 1-methyl-3-butylimidazolium bromide in methanol, add NaHSO 4 Aqueous solution with a content of 1mol was stirred and reacted at room temperature for 24h. Then suction filtration, the filter...
preparation Embodiment 3
[0046] Synthesis of IL-3 as Catalyst of N-Butylpyridine Trifluoromethanesulfonate-Pyrophosphoric Acid-Dodecylbenzenesulfonate Catalyst
[0047] In a three-necked flask, add 1 mol of pyridine and 1.05 mol of 1-chlorobutane, pass through N 2 After purging for 20mim, start stirring and heat to 75°C for 30-36h. After the reaction was completed, it was left to cool down to room temperature, the lower layer of the solution was light yellow, and the upper layer was unreacted raw materials. The upper layer liquid was decanted, 3 times the volume of diethyl ether was added to the lower layer liquid to wash, and then the diethyl ether was separated to remove unreacted raw materials. After washing, dry at 70°C for 24 hours to obtain light yellow viscous N-butylpyridinium chloride salt.
[0048] Mix the obtained N-butylpyridinium chloride salt and 1mol trifluoromethanesulfonic acid in a three-necked flask, stir at 50°C for 24 hours, extract and purify with ether, then spin to remove the...
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