A kind of synthesis technology of new jasmine aldehyde
A Xinyang jasmonal and synthetic process technology, applied in the direction of organic chemistry, can solve the problems of low product yield and purity, difficult recovery of catalysts, easy discoloration of products, etc., and achieve less reaction by-products, stable finished products, and low cost Effect
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Embodiment 1
[0034] A kind of synthetic technique of new ocean jasmonal, comprises the following steps:
[0035] (1) Alcoholysis reaction: at a certain temperature, add alcohol to Xinyang jasmonal monoester, use potassium carbonate as a catalyst, and remove the solvent after the reaction is complete to obtain the Xinyang jasmonal crude product;
[0036] (2) Refining of the crude product: the Xinyang jasmonal crude product obtained in the step (1) is subjected to steps including washing and distillation to obtain the finished product of Xinyang jasminal;
[0037] Wherein, in the alcoholysis reaction of step (1), the removed solvent is hydrolyzed in an alkaline catalyst solution at 40-50°C to separate the alcohol, and the alcohol is used for the alcoholysis reaction with Xinyang jasmonal monoester, The content of water in the alcohol accounts for 0-30% by weight of the whole reaction system.
[0038] Adopt above-mentioned synthesis process to synthesize Xinyangjasmonal, concrete reaction co...
Embodiment 2
[0044] Adopt the synthetic technique of embodiment one to synthesize new foreign jasmonal, concrete reaction condition is: the temperature of step (1) alcoholysis reaction is 30-40 ℃, the alcohol of alcoholysis reaction is methyl alcohol, according to the alcoholysis reaction of step (1) 5 comparative examples are set and numbered respectively according to the different amounts of catalysts. The amount of catalysts is based on the molar weight of Xinyang jasmonal monoester: 0.01-0.1mol (a), 0.1-0.2mol (b), 0.2-0.4mol ( c), 0.4-0.5mol (d), 0.5-1mol (e).
[0045] The products obtained after the reaction were sampled and detected by LC / MS to obtain the yield, purity and reaction time of the finally synthesized Xinyang Jasmonal. The experimental data are shown in Table 2.
[0046] Table 2 Example 2 Xinyang jasmonal detection data results
[0047]
[0048] a
[0049]As can be seen from the above data, the yield of Xinyang jasmonal in the range of catalyst consu...
Embodiment 3
[0051] Adopt the synthesis process of Example 1 to synthesize Xinyangjasmonal, and the specific reaction conditions are: the temperature of the alcoholysis reaction in step (1) is 30-40°C, and the amount of catalyst is 0.2-0.4mol based on the molar weight of Xinyangjasmonal monoester According to step (1) alcoholysis reaction adopts the difference of solvent to set 5 contrast examples and number respectively, be respectively methyl alcohol (1), ethanol (2), tert-butanol (3), ethylene glycol (4), toluene ( 5).
[0052] The products obtained after the reaction were sampled and detected by LC / MS to obtain the yield, purity and reaction time of the finally synthesized Xinyang Jasmonal. The experimental data are shown in Table 3.
[0053] Table 3 Example Sanxinyang jasmonal detection data results
[0054]
[0055] 4
[0056] From the above data, it can be known that different solvents are used as solvents for alcoholysis reaction, and the yields of Xinyangjasmo...
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