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Method for preparing sandaler

The technology of a kind of sandalwood ether and preparation steps is applied to the green process route of synthesizing sandalwood ether, and the preparation field of sandalwood ether can solve the problems of poor hydrogenation selectivity, high equipment requirements and high catalyst price, and achieves improvement of synthesis process. Effect

Inactive Publication Date: 2010-12-08
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) In industry, this step of epoxidation mainly adopts organic peracid as epoxidation reagent, such as peracetic acid (US2838524), m-chloroperoxybenzoic acid (J.Org.Chem., 1975,40, 2259), etc., this type of catalyst is expensive and highly corrosive. After the reaction, a large amount of acid will be produced, polluting the environment, and the yield is low.
[0005] (2) The hydrogenation reaction requires hydrogenation in an autoclave, which requires high equipment, poor hydrogenation selectivity, and difficult separation of the produced product and by-products

Method used

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  • Method for preparing sandaler

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Embodiment 1

[0028] (1), Synthesis of 3,7-dimethyl-7-methoxyoctene

[0029] At room temperature, 405ml (10.0mol) of methanol was added in a 1000ml three-necked round-bottomed flask, and 182ml of dihydromyrcene (industrial product, content about 85%, 1.0mol) was added dropwise under stirring, and 22ml of concentrated sulfuric acid (content greater than 1.0mol) was slowly added dropwise. 98%, 0.4mol), after feeding, the temperature was raised to 65°C and refluxed for 5 hours, then cooled to room temperature, washed with water, and the organic layer was separated and washed with 5% NaHCO 3 The aqueous solution was washed to neutrality, and the obtained organic layer was subjected to vacuum distillation to reclaim 22.8 g of dihydromyrcene as a raw material (recyclable), and collected product fraction 3,7-dimethyl-7-methoxyoctene 115.7 g g (gas phase content is 96.9%), productive rate is 81.3%;

[0030] (2), synthesis of 3,7-dimethyl-7-methoxy-1,2-epoxyoctane

[0031] Catalysts for epoxidatio...

Embodiment 2

[0036] (1), Synthesis of 3,7-dimethyl-7-methoxyoctene

[0037] At room temperature, 324ml (8.0mol) of methanol was added in a 1000ml three-necked round-bottomed flask, and 182ml of dihydromyrcene (industrial product, content about 85%, 1.0mol) was added dropwise under stirring, and 22ml of concentrated sulfuric acid (content greater than 1.0mol) was slowly added dropwise. 98%, 0.4mol), after feeding, the temperature was raised to 65°C and refluxed for 5 hours, then cooled to room temperature, washed with water, and the organic layer was separated and washed with 5% NaHCO 3 The aqueous solution was washed to neutrality, and the obtained organic layer was subjected to vacuum rectification to recover 47.6 g of dihydromyrcene as a raw material (recyclable), and 92.0 g of product fraction 3,7-dimethyl-7-methoxyoctene was collected. g (gas phase content is 96.5%), productive rate is 82.4%;

[0038] (2), synthesis of 3,7-dimethyl-7-methoxy-1,2-epoxyoctane

[0039] Catalysts for epo...

Embodiment 3

[0044] (1), Synthesis of 3,7-dimethyl-7-methoxyoctene

[0045] At room temperature, 486ml (12.0mol) of methanol was added in a 1000ml three-neck round-bottomed flask, and 182ml of dihydromyrcene (industrial product, content about 85%, 1.0mol) was added dropwise under stirring, and 22ml of concentrated sulfuric acid (content greater than 1.0mol) was slowly added dropwise. 98%, 0.4mol), after feeding, the temperature was raised to 65°C and refluxed for 5 hours, then cooled to room temperature, washed with water, and the organic layer was separated and washed with 5% NaHCO 3 The aqueous solution was washed to neutrality, and the obtained organic layer was subjected to vacuum distillation to recover 22.3 g of dihydromyrcene (recyclable) as the raw material, and 119.1 g of product fraction 3,7-dimethyl-7-methoxyoctene was collected. g (gas phase content is 96.7%), productive rate is 83.4%;

[0046] (2), synthesis of 3,7-dimethyl-7-methoxy-1,2-epoxyoctane

[0047] Catalysts for ep...

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Abstract

The invention relates to a method for preparing sandaler. The method comprises the following steps of: performing methoxylation on industrial grade dihydromyrcene serving as a raw material; performing epoxidation on the methoxylation product; and performing hydrogenation reduction on the epoxidation product to obtain the sandaler. The epoxidation in the method for preparing the sandaler has the advantages of mild reaction conditions, simple and practical reaction process, no byproduct, simple after-treatment and high efficiency and selectivity; and the hydrogenation reduction in the method for preparing the sandaler has the advantages of low equipment requirement, mild reaction conditions, safe operation, high catalytic activity, high selectivity, wherein the selectivity of the sandaler is over 97 percent.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a preparation method of santalyl ether, in particular to a green process route for synthesizing santalyl ether. Background technique [0002] Sandalwood is an important single fragrance, which is used in a large amount in various flavor types of daily chemical essences. It is widely used in many fields such as daily chemicals, decoration, gifts, etc., especially in incense essences. The amount used is so high that synthetic sandalwood has become very important due to the depletion of natural resources. Synthetic santalaceae include two categories of santalyl ether and santalol. Sandalyl ether is an acyclic compound with methoxyl and alcoholic hydroxyl groups. It has stable chemical properties and will not cause discoloration. It has a strong and pleasing aroma of sandalwood and flowers. It was first listed by the British B.B.A company and named Osyrol . Sandalyl ether ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/13C07C41/26
CPCY02P20/584
Inventor 王伟邱红赵冰高妍姚红果
Owner SHANGHAI INST OF TECH
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