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Preparation method of 2,6-dimethyl-6-alkyloxy(or hydroxyl)heptaldehyde

A technology of alkoxy and dimethyl, which is applied in the field of preparation of 2,6-dimethyl-6-alkoxy (or hydroxy) heptanal, which can solve environmental pollution, high equipment requirements, cumbersome steps, etc. problems, to achieve the effect of good industrial reliability, low separation difficulty and simple process

Active Publication Date: 2014-05-28
NANJING ENETEKS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The steps of these methods are cumbersome, the product yield is low, protection and deprotection groups are required, and the recovery of the protection groups is difficult, ethyl chloroacetate is more harmful to aquatic organisms, and the use of strong acids and strong bases requires higher equipment. And it is easy to pollute the environment, so it is not suitable for use in modern industrial production

Method used

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  • Preparation method of 2,6-dimethyl-6-alkyloxy(or hydroxyl)heptaldehyde
  • Preparation method of 2,6-dimethyl-6-alkyloxy(or hydroxyl)heptaldehyde
  • Preparation method of 2,6-dimethyl-6-alkyloxy(or hydroxyl)heptaldehyde

Examples

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Embodiment 1

[0036] A preparation method of 2,6-dimethyl-6-hydroxyl-heptanal, comprising the steps of:

[0037] (1) Ozonation reaction of dihydromyrcenol (2,6-dimethyl-2-hydroxy-7-octene)

[0038] Take 22kg of dihydromyrcenol, 44kg of solvent xylene, and 44kg of water in a 150L bubble column reactor (height-to-diameter ratio 10:1), 1.5m from the bottom of the reactor 3 The speed of / h / (kg raw material) is slowly passed into O 3 The mole percentage is 10% O 3 / O 2 The reaction temperature of the mixture is 10°C. After the ozonation reaction occurs for 2 hours, use KI test paper to test the gas at the outlet of the reactor. The KI test paper turns blue. After the material is discharged from the bottom of the reactor, it is separated by a phase separator, and the oil phase is taken out. 58kg of dihydromyrcenol ozonation product is stored in a storage tank, filled with nitrogen for protection.

[0039] (2) Reduction reaction of dihydromyrcenol (2,6-dimethyl-2-hydroxy-7-octene) ozonation pr...

Embodiment 2

[0042] A preparation method of 2,6-dimethyl-6-methoxy-heptanal, comprising the steps of:

[0043] (1) Ozonation reaction of dihydromyrcene methyl ether (2,6-dimethyl-2-methoxy-7-octene)

[0044] Take 260g of dihydromyrcene methyl ether, 130g of solvent acetonitrile, and 260g of water in a 1L bubble column reactor (height-to-diameter ratio 10:1). 3 The speed of / h / (kg raw material) is slowly passed into O 3 The mole percentage is 8% O 3 / O 2 The reaction temperature of the mixture is 12°C. After the ozonation reaction occurs for 3.5 hours, use the KI test paper to test the gas at the gas outlet of the reactor. The KI test paper turns blue, and continue to pass O 3 / O 2 After the mixture was reacted for 1 hour, the material was transferred from the reactor to a separatory funnel, and 370 g of the ozonated product of dihydromyrcene methyl ether in the oil phase was taken out and stored in a bottle under nitrogen protection.

[0045] (2) Reduction reaction of dihydromyrcene m...

Embodiment 3

[0048] A preparation method for 2,6-dimethyl-6-acetoxy-heptanal, comprising the steps of:

[0049] (1) Ozonation reaction of dihydromyrcenyl acetate (2,6-dimethyl-2-acetoxy-7-octene)

[0050] Take 520g of dihydromyrcenyl acetate, 260g of acetonitrile as a solvent, and 520g of water in a 2L bubble column reactor (height-to-diameter ratio 8:1). 3 The speed of / h / (kg raw material) is slowly passed into O 3 The molar percentage is 7% O 3 / O 2 The reaction temperature of the mixture is 11°C. After the ozonation reaction occurs for 4 hours, use the KI test paper to test the gas at the outlet of the reactor. The KI test paper turns blue, and continue to pass O 3 / O 2 After the mixture was reacted for 1 h, the material was transferred from the reactor to a separatory funnel, and 740 g of the ozonated product of dihydromyrcenyl acetate in the oil phase was taken out and stored in a bottle under nitrogen protection.

[0051] (2) Reduction reaction of 2,6-dimethyl-2-acetoxy-7-octene...

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PUM

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Abstract

The invention relates to a preparation method of 2,6-dimethyl-6-alkyloxy(or hydroxyl)heptaldehyde, comprising the following steps: Step 1, placing 2,6-dimethyl-2-alkyloxy(or hydroxyl)-7-octene, a solvent and water in a reactor, blowing a O3 / O2 mixture into the reactor, layering products after the reaction, and blowing a protective gas into an oil phase for protection; Step 2, adding a bisulfite or pyrosulfite solution into the oil phase obtained from the Step 1, heating, neutralizing products obtained after the reaction by the use of an alkaline solution, separating to obtain oil and water phases, washing the oil phase to neutral, and separating to obtain oil and water phases. The oil phase obtained is a crude product 2,6-dimethyl-6-alkyloxy(or hydroxyl)heptaldehyde. The preparation method provided by the invention has advantages of simple process, high conversion rate of raw materials, high product yield, low follow-up separation difficulty, good industrial reliability, is environmentally friendly, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of spices, in particular to an important derivative of melon aldehyde, and more specifically to a preparation method of 2,6-dimethyl-6-alkoxy (or hydroxyl) heptanal. Background technique [0002] 2,6-Dimethyl-6-alkoxy (or hydroxy) heptanal (hereinafter referred to as heptanal), whose structural formula is shown in formula (3), is an important derivative of melon aldehyde. [0003] [0004] R is H, methyl, ethyl, acetyl, propyl, isopropyl, butyl, isobutyl, pentyl, 1-hydroxy-2-methyl-1-propyl, isopentyl, cyclopentyl One of radical, n-hexyl or allyl. [0005] It enhances the floral or aromatic scent of perfume or other cosmetic products. Such as 2,6-dimethyl-6-hydroxyheptanal, which has the aroma of melon, tropical fruit, raspberry, lily-of-the-valley, and can be used as an additive in tobacco, food, detergent, soap, fabric softener, perfume, etc. ; Another example is 2,6-dimethyl-6-methoxyheptanal, which is a colo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/14C07C47/19C07C47/198C07C45/59C07C67/297
CPCC07C67/293C07C45/40C07C2601/08C07C47/19C07C47/198C07C69/14C07C67/297C07D323/02
Inventor 杨高东林力克王宝荣周政张志炳
Owner NANJING ENETEKS
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