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Preparation method of fenchone

A fenone and solution technology, applied in the field of organic compound preparation, can solve the problems of low reaction conversion rate of potassium permanganate, large amount of sodium hypochlorite solution, difficulty in distinguishing between oil layer and water layer, etc., and achieves low price, easy operation and conversion. high rate effect

Inactive Publication Date: 2015-12-16
南宁辰康生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Existing research application shows: sodium hypochlorite has higher conversion rate, but sodium hypochlorite is easy to deteriorate and is not easy to preserve, and in actual operation, the amount of sodium hypochlorite solution is large, resulting in very low equipment utilization rate; potassium permanganate reaction conversion rate is not high; Potassium dichromate can also be used as a catalyst to obtain a good conversion rate, but the reaction solution is dark green, and it is very difficult to distinguish the oil layer from the water layer, which is not conducive to production operations, and the amount of waste water is large, which is likely to cause environmental pollution

Method used

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  • Preparation method of fenchone
  • Preparation method of fenchone

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preparation example Construction

[0020] The embodiment of the present invention provides a kind of preparation method of fenchone, comprises the following steps:

[0021] S1. Weigh 65-85% of fenchol (purity 95%-98%), 0.5-5% of self-made dehydrogenation catalyst, and 10-25% of organic solvent by weight percentage;

[0022] S2. Put the fecundol and organic solvent weighed in step S1 in a three-necked flask, stir, and heat the material in an oil bath to reflux, remove a small amount of water in the material, and obtain solution A;

[0023] S3. Stop heating the solution A obtained in step S2 in the oil bath, wait until the temperature of the kettle (oil temperature) drops below 170°C, stop stirring, add the self-made catalyst weighed in step S1, turn on the stirring, and heat the reaction solution to the reflux temperature. Dehydrogenation reaction, the reaction time is 5 to 7 hours, to obtain solution B;

[0024] S4, the solution B obtained in step S3 is distilled out of solvent and organic solvent to obtain so...

Embodiment 1

[0040] A preparation method of fenchone, comprising the steps of:

[0041] S1. Weigh 75% of fenchol (95% purity) by weight, 3% of self-made dehydrogenation catalyst, and 15% of organic solvent;

[0042] S2. Put the fecundol and the organic solvent weighed in step S1 in a three-necked flask, stir, and heat the material in an oil bath to reflux, remove a small amount of water in the material, and obtain solution A;

[0043] S3, stop the oil bath heating of the solution A obtained in step S2, wait until the temperature of the kettle (oil temperature) drops to 170°C, stop stirring, add the self-made catalyst weighed in step S1, turn on the stirring, heat the reaction solution to the reflux temperature for degassing Hydrogen reaction, the reaction time is 5 hours, to obtain solution B;

[0044] S4, the solution B obtained in step S3 is distilled out of solvent and organic solvent to obtain solution C;

[0045] S5. Add the solution C obtained in step S4 into a fractionation still,...

Embodiment 2

[0051] A preparation method of fenchone, comprising the steps of:

[0052] S1. Weigh 80% of fenchol (95% purity) by weight, 2% of self-made dehydrogenation catalyst, and 18% of organic solvent;

[0053] S2. Put the fecundol and the organic solvent weighed in step S1 in a three-necked flask, stir, and heat the material in an oil bath to reflux, remove a small amount of water in the material, and obtain solution A;

[0054] S3, stop the oil bath heating of the solution A obtained in step S2, wait until the temperature of the kettle (oil temperature) drops to 165 ° C, stop stirring, add the self-made catalyst weighed in step S1, turn on the stirring, heat the reaction solution to the reflux temperature for degassing Hydrogen reaction, the reaction time is 7 hours, to obtain solution B;

[0055] S4, the solution B obtained in step S3 is distilled out of solvent and organic solvent to obtain solution C;

[0056] S5. Add the solution C obtained in step S4 into a fractionation stil...

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Abstract

The invention provides a preparation method of fenchone. The preparation method has the beneficial effects that fenchone is prepared by dehydrogenating fenchol by adopting a self-made dehydrogenation catalyst; fenchone has high conversion rate and good selectivity; the reaction process is mild; a nontoxic and harmless plant-derived organic solvent is adopted, thus reducing the residues of toxic and harmful substances, and the solvent can be also recycled; the preparation method has the characteristics of high yield, high finished product purity, simple process, easiness in operation, abundant raw material sources and low cost.

Description

technical field [0001] The invention is applicable to the field of preparation of organic compounds, and in particular relates to a preparation method of fenchone. Background technique [0002] The chemical name of fenchone is (1R,4S)-1,3,3-trimethyl-bicyclo[2,2,1]heptane-2-one, also known as fennelone, fennelone, 1 , 3,3-Trimethyl-2-norbornanone. The English name is 1,3,3-trimethylbicyclo[2.2.1]heptan-2-one, Fenchone; CasNo.: 1195-79-5, EINECSNo.: 214-804-6, molecular formula: C 10 h 16 O; Molecular weight: 152.23; Melting point: 5~6℃101.325kPa; Boiling point: 193~194℃101.325kPa; Flash point (TCC): 60℃; Refractive index: 1.460~1.46320℃; Density: 0.938~0.94825℃. Fenchone is a colorless to pale yellow oily liquid, soluble in ethanol and non-volatile oil, insoluble in propylene glycol, and extremely insoluble in water (solubility in water is 744mg / L at 25°C). [0003] Natural products exist in cumin, arborvitae, etc. [0004] Fenketone has cool fragrance, camphor and mint...

Claims

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Application Information

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IPC IPC(8): C07C45/29C07C45/82C07C49/437
CPCC07C45/29C07C45/82C07C49/437
Inventor 何春茂邓倩李华杰
Owner 南宁辰康生物科技有限公司