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Method for synthesizing racemic sclareolide

A technology for the synthesis of sclareolide and its synthesis method, which is applied in the field of synthesis of racemic sclareolide, can solve the problems of environmental pollution and difficulty in reusing, and achieve the effects of being environmentally friendly, easy to operate, and suitable for industrial production

Inactive Publication Date: 2012-02-15
北京安胜瑞力科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004]The current common synthesis method of racemic sclareolide is to use 4-methyl-6-(2,6,6-trimethyl-1-cyclo Hexenyl)-3-hexene-1-acid (referred to as hexadecanoic acid) as raw material, in toluene, nitromethane, dichloromethane and other solvents, in chlorosulfonic acid (JP05186453), stannous chloride (US4503240 ), trifluoroacetic acid (EP165458, Agric Biol Chem 50 (6) 1475~1480, 1986) catalyzed cyclization, and the acidic catalyst used in the reaction process needs to be washed away with water at last, causing environmental pollution and being difficult to reuse

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Add SO to a 100ml four-necked bottle 4 2- / ZrO 2 Type solid superacid catalyst 1g;

[0020] (2) Add 10ml of anhydrous toluene;

[0021] (3) Introduce nitrogen gas into the reactor at a flow rate of 2ml / min;

[0022] (4) Heating, raising the temperature to 112 degrees, refluxing for 1 hour, steaming the toluene, then raising the temperature to 220 degrees, and keeping it for 1 hour;

[0023] (5) Cooling down, nitrogen flow down to 25 degrees, stop nitrogen;

[0024] (6) Add 60 ml of anhydrous toluene, 4-methyl-6-(2,6,6-trimethyl-1-cyclohexenyl)-3-hexene-1-oic acid (hexadecanoic acid) 1 gram;

[0025] (7) Heating, raising the temperature to 115 degrees, stirring and reacting for 6 hours, sampling and monitoring until the raw material is less than 1%;

[0026] (8) Filter and recover 1 gram of catalyst;

[0027] (9) Precipitate the mother liquor to half the volume by rotary evaporation, cool to -10 degrees, and let stand;

[0028] (10) Filter and dry the residu...

Embodiment 2

[0033] (1) Add SO to a 250ml stainless steel reactor 4 2- / Fe 2 o 3 Type solid superacid catalyst 3g;

[0034] (2) Add 50 ml of anhydrous xylene;

[0035] (3) Introduce nitrogen gas into the reactor at a flow rate of 4ml / min;

[0036] (4) Heating, raising the temperature to 130°C, refluxing for 2 hours, steaming the xylene, then raising the temperature to 220°C, and keeping it for 2 hours;

[0037] (5) Cooling down, nitrogen flow down to 20 degrees, stop nitrogen;

[0038] (6) Add 150 ml of anhydrous tetrahydrofuran, 4-methyl-6-(2,6,6-trimethyl-1-cyclohexenyl)-3-hexene-1-oic acid (hexadecanoic acid) 3 gram;

[0039] (7) Heating, raising the temperature to 75 degrees, stirring and reacting for 12 hours, sampling and monitoring until the raw material is less than 1%;

[0040] (8) Filter and recover 3 grams of catalyst;

[0041] (9) Precipitate the mother liquor to half of its volume by rotary evaporation, cool to 10 degrees, and let stand;

[0042] (10) Filter and dry ...

Embodiment 3

[0047] (1) Add SO to a 500ml four-necked bottle 4 2- / SnO 2 –Al 2 o 3 5 grams of solid superacid catalysts; (2) add 100 milliliters of anhydrous xylene;

[0048] (3) Introduce nitrogen gas into the reaction kettle at a flow rate of 6ml / min;

[0049](4) Heating, raising the temperature to 130 degrees, refluxing for 3 hours, steaming the xylene, then raising the temperature to 220 degrees, and keeping it for 2 hours;

[0050] (5) Cooling down, nitrogen flow down to 40 degrees, stop nitrogen;

[0051] (6) Add 300 ml of anhydrous xylene, 4-methyl-6-(2,6,6-trimethyl-1-cyclohexenyl)-3-hexene-1-oic acid (hexadecanoic acid) 5 grams;

[0052] (7) Heating, raising the temperature to 130 degrees, stirring and reacting for 4 hours, sampling and monitoring until the raw material is less than 1%;

[0053] (8) 5 grams of catalyst were recovered by filtration;

[0054] (9) Precipitate the mother liquor to half of its volume by rotary evaporation, cool to 20 degrees, and let stand; ...

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PUM

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Abstract

The invention belongs to the technical field of daily use chemicals, and discloses a method for synthesizing racemic sclareolide. The synthetic method comprises the step of: making 4-methly-6-(2,6,6-trimethyl-1-cyclohexenyl)-3-hexene-1-acid serving as a raw material react with a solid super acid serving as a catalyst in an organic solvent to obtain racemic sclareolide. The method for synthesizing the racemic sclareolide is environmentally-friendly, is easy to operate, and has high yield; and the catalyst used in the synthetic method can be used repeatedly, so that the production cost is lowered, and the method is more suitable for industrial production.

Description

Technical field [0001] The present invention is a daily chemical technology field, which involves a synthesis method of girosp -ciaolinel. Background technique [0002] Smooth incense perilla isolate, mainly used as a natural ambergris fragrant supplies -the synthetic raw materials of the anti -spin corache ether.The substitute for the raw materials of the raw materials of the arax fragrance of the scent, the commodity name Cetalox.It is widely used in high -grade perfumes and cosmetics fragrances, which is very suitable for skin, hair and fabrics with fragrance spices.Frequent soap, cream, cream, and fragrance are used for fragrance and fragrant incense.Sleeping perilla beext is saponic and restored. [0003] At the same time, the incense perilla beef has excellent tobacco -flavored fragrant agent. In mixed cigarettes, it can cover the coarse and miscellaneous gas of tobacco, to improve and improve the quality of fragrance, give the tobacco pleasant characteristic aroma, and mak...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/92
Inventor 朱伟文袁西福谌湘毅蔺楠
Owner 北京安胜瑞力科技有限公司
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