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Synthetic method of dihydrogen geranyl acetone and dihydrogen nicky acetone

A technology of dihydrogeranyl acetone and dihydrofarnesyl acetone, which is applied in the field of Carroll reaction, can solve problems not involving the synthesis method of dihydrogeranyl acetone or dihydrofarnesyl acetone, and reduce the Production cost, high efficiency, effect of avoiding pollution

Active Publication Date: 2014-04-30
JILIN BEISHA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] CN1894190A (2007-1-10) discloses a kind of production method of tetrahydrogeranyl acetone, but does not relate to the synthetic method of dihydrogeranyl acetone or dihydrofarnesyl acetone

Method used

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  • Synthetic method of dihydrogen geranyl acetone and dihydrogen nicky acetone
  • Synthetic method of dihydrogen geranyl acetone and dihydrogen nicky acetone
  • Synthetic method of dihydrogen geranyl acetone and dihydrogen nicky acetone

Examples

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Embodiment 1

[0051] Synthesis of dihydrogeranylacetone: 5000L stainless steel reaction kettle, add 1000kg of dihydrolinalool, add 30kg of aluminum isopropoxide as a catalyst, add 770kg of methyl acetoacetate dropwise at about 180°C, and complete the dropwise addition in about 2.5 hours After adding methyl acetoacetate dropwise, continue the heat preservation reaction for about 2 hours. As the reaction progresses, carbon dioxide and methanol gas continue to overflow from the reaction system, pass through the cooling tower and film cooler, and enter the gas-liquid separator to separate a large amount of methanol , carbon dioxide gas carries a small amount of acetone and low-boiling substances into the decarbonylation furnace for combustion and then converts carbon dioxide and water. The carbon dioxide gas with a purity of more than 99% is separated through the separator, and then enters the alkynylation station through the gas guide pipe to adjust the pH value of the water phase. . The end p...

Embodiment 2

[0060] Synthesis of dihydrofarnesylacetone: 5000L stainless steel reaction kettle, add 1000kg of tertiary nerolidol, add 27 kg of aluminum isopropoxide as catalyst, add 540kg of methyl acetoacetate dropwise at about 180°C, drop for about 2.5 hours After the addition is completed, add the methyl acetoacetate dropwise and continue the heat preservation reaction for about 2 hours. As the reaction progresses, carbon dioxide and methanol gas continuously overflow from the reaction system, pass through the cooling tower and film cooler, and enter the gas-liquid separator to separate a large amount of Methanol, carbon dioxide gas with a small amount of acetone and low-boiling substances enters the decarbonylation furnace for combustion and converts carbon dioxide and water. The carbon dioxide gas with a purity of more than 99% is separated through a separator, and then enters the alkynylation station through the gas guide pipe to adjust the water phase. pH value. The end point of the...

Embodiment 3

[0066] The synthetic method of dihydrogeranyl acetone comprises steps:

[0067] (1) Ingredients: Weigh 800 parts of dihydrolinalool, 25 parts of aluminum isopropoxide, and 700 parts of methyl acetoacetate by weight, and set aside;

[0068] (2) Synthesis: Mix all the dihydrolinalool and aluminum isopropoxide, raise the temperature to 160°C and start to add methyl acetoacetate dropwise, after the dropwise addition, continue to keep warm for 1.5h to synthesize dihydrogeranylacetone;

[0069] (3) Recovery of by-products: Cool and separate the carbon dioxide and methanol gas generated during the reaction, recover the methanol liquid generated by cooling, and introduce the carbon dioxide gas entrained with methanol gas and low-boiling organic impurity gas into the decarbonylation furnace, of which methanol Gas and low-boiling organic impurity gas are fully burned in the decarbonylation furnace to generate carbon dioxide and water vapor. The mixed gas is then separated and converted ...

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Abstract

The invention relates to a Carroll reaction, and particularly relates to a synthetic method of dihydrogen geranyl acetone and dihydrogen nicky acetone. The method comprises the following steps: reacting dihydro linalool or dihydrogen nerolidol taken as a raw material and aluminium isopropoxide taken as a catalyst with methyl acetoacetate or ethyl acetoacetate to generate the dihydrogen geranyl acetone or dihydrogen nicky acetone, simultaneously generating carbon dioxide and methyl alcohol for treatment. The synthetic method is high in reaction yield, and high in purity, a by-product methanol can be fully recovered, environmental pollution is avoided, production is energy-saving and environment-friendly, meanwhile, the production cost is reduced, a carbon dioxide gas containing a little amount of methanol gas and low-boiling organic impurity gas enters a decarburization furnace to combust in by-product recovery, and the generated heat energy can be supplied to decarboxylic reaction in synthesis, so that heat cyclic utilization is achieved. The collected carbon dioxide is high in purity, and can be directly supplied to the required post, emission of atmosphere is reduced, production is energy-saving and environment-friendly, and meanwhile, the production cost is reduced.

Description

technical field [0001] The invention relates to a Carroll reaction, in particular to a synthesis method of dihydrogeranylacetone and / or dihydrofarnesylacetone. Background technique [0002] Dihydrogeranylacetone is a very important pharmaceutical and chemical intermediate. It can be used to prepare geranium oil and food flavors. It is widely used in the field of flavors and fragrances. More importantly, dihydrogeranylacetone and dihydrofarnesylacetone It is an important intermediate for the synthesis of vitamin E side chain isophytic alcohol. Since vitamin E was discovered, it has been widely used in the fields of medicine, health care medicine, feed additives and food additives, because of its ability to improve the body's own immunity and Promote metabolism and other effects, and at the same time have effects such as prolonging aging. Therefore, the synthesis technology of dihydrogeranylacetone and dihydrofarnesylacetone has attracted people's attention. [0003] CN189419...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/203C07C45/65C07C31/04C07C29/00
CPCC07C29/00C07C45/65C07C49/203C07C31/04Y02A50/20Y02P20/10Y02P20/52
Inventor 黄升洪树良赵新颖
Owner JILIN BEISHA PHARMA
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