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Method for synthesizing karanal

A technology of carrageenaldehyde and synthesis method, applied in the direction of organic chemistry and the like, can solve the problems of low yield and the like, and achieve the effects of wide sources, low cost and reasonable design

Inactive Publication Date: 2013-06-19
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of the blank of the complete synthesis method of caralalin in the prior art, and the lower problem of the obtained yield, the present invention designs a scientific and rational synthetic route of caralinal

Method used

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  • Method for synthesizing karanal
  • Method for synthesizing karanal

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preparation example Construction

[0012] A complete synthesis method of caralanal is provided, and the specific synthesis route is divided into three steps:

[0013] (1) Synthesis of intermediate (I) 2-methyl-2-sec-butyl-diethyl malonate: Add 0.33g-0.66g sodium metal to 25mL-80mL absolute ethanol, and wait for the metal Add 2.11g-4.17g diethyl 2-methylmalonate after complete reaction of sodium, stir and reflux for 30min-50min, add 2.49g-4.95g 2-bromobutane, and reflux at 80-90℃ React for 4h-5h. After the reaction is over, cool the reaction mixture to room temperature, distill off the solvent ethanol, add 1-3 times the volume of the mixture to dilute with water, and then extract 3 times with diethyl ether that is 1-3 times the volume of the diluted liquid, and combine the extractions liquid, and the extract was washed twice with distilled water and saturated NaCl aqueous solution, dried to remove water, and filtered to remove impurity NaCl, distilled ether in the filtrate to obtain 2-methyl-2-sec-butyl-propaned...

Embodiment 1

[0017] (1), the synthesis of intermediate (I) 2-methyl-2-sec-butyl-diethyl malonate:

[0018] Weigh 0.33g of sodium metal and slowly put it into a 50mL three-necked bottle (room temperature) filled with 25mL of absolute absolute ethanol. After all the sodium has reacted, 2.11g of diethyl 2-methylmalonate was slowly added dropwise with a constant pressure dropping funnel, stirred and refluxed for 30min, and then 2.49g of 2-bromobutane was slowly added dropwise. , reflux reaction 4h, during the reaction, track the reaction process with GC and TLC;

[0019] After the reaction, the reaction mixture was cooled to room temperature, the solvent ethanol was distilled off, and an equal volume of the mixture was added to dilute with water, and then extracted three times with an equal volume of dilute liquid ether. After combining the extracts, they were washed with distilled water and saturated NaCl aqueous solution respectively. Extract the solution twice, dry and remove the moisture ...

Embodiment 2

[0026] (1), the synthesis of intermediate (I) 2-methyl-2-sec-butyl-diethyl malonate:

[0027] Weigh 0.50g of sodium metal and slowly put it into an 80mL three-necked bottle (room temperature) filled with 50mL of absolute absolute ethanol. After all the sodium has reacted, slowly drop 3.10g of 2-methyldiethylmalonate into it with a constant pressure dropping funnel, stir and reflux for 40min, then slowly add 3.83g of 2-bromobutane dropwise, at 85°C, reflux Reaction 4.5h, during the reaction, track the reaction process with GC and TLC;

[0028]After the reaction, the reaction mixture was cooled to room temperature, the solvent ethanol was evaporated, diluted with water twice the volume of the mixture, extracted three times with diethyl ether twice the volume of the diluted liquid, and the combined extracts were washed with distilled water and saturated NaCl aqueous solution respectively. 2 times, dry to remove water, filter to remove impurity NaCl, and distill off the ether in ...

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Abstract

The invention discloses a method for synthesizing karanal, relating to the synthesis of organic compounds. The method comprises the following steps of: with 2-diethyl methylmalonate as a raw material, carrying out alkylation reaction on 2-butyl bromide and the 2-diethyl methylmalonate to synthesize 2-methyl-2-sec-butyl-diethyl malonate as an intermediate (I); with the obtained 2-methyl-2-sec-butyl-diethyl malonate as a raw material, carrying out reduction reaction on the 2-methyl-2-sec-butyl-diethyl malonate through metal sodium and absolute ethanol to synthesize 2-methyl-2-sec-butyl-1,3 propanediol as an intermediate (II); with the obtained 2-methyl-2-sec-butyl-1,3 propanediol as a raw material, carrying out condensation reaction on 3, 5-dimethyl-4-cycolhexene formaldehyde and the 2-methyl-2-sec-butyl-1,3 propanediol to obtain the karanal product. According to the invention, a complete karanal synthesis route is designed, so that the yield of the karanal product is increased; and thesynthesis route provided by the invention is reasonable in design, the raw materials are acquired widely and easily, the synthesis reaction is simple and easy to perform, the cost is lower and the industrial production is easy to realize.

Description

technical field [0001] The invention relates to a method for synthesizing organic compounds, in particular to a method for synthesizing carragenal. Background technique [0002] Carla flower aldehyde is an artificial fragrance, its structure has not been found in nature, it has a strong and gorgeous woody and amber aroma, and the aroma is extremely long-lasting. Carla flower aldehyde is mainly used in the formulation of daily chemical essence. It can be used as a functional amber fragrance in the head fragrance to the tail fragrance. Because of the strong persistence of the fragrance in the formula, it should not be used in excess. It can play a decisive role, and the dosage is generally 10% or 1% of the diluent, which has a good fragrance retention effect on fabrics. About the synthetic method of carla flower aldehyde, do not see relevant bibliographical information at present at home, and abroad Anglo-Dutch Quest company produces carla flower aldehyde with privet aldehyde...

Claims

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Application Information

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IPC IPC(8): C07D319/06
Inventor 尹卫平邓瑞雪张志新赵爽刘普
Owner HENAN UNIV OF SCI & TECH
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