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Leaf alcohol synthesis method

A synthetic method and technology of leaf alcohol, which is applied in the field of high-grade flavor and fragrance leaf alcohol, can solve the problems of high production cost, dependence on import of products, failure of industrialization, etc., and achieve the effect of low cost

Inactive Publication Date: 2006-04-26
大连圣迈化学有限公司 +1
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  • Abstract
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  • Claims
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Problems solved by technology

[0007] In China, there were several units engaged in the research on the synthesis of leaf alcohol, but none of them could be industrialized. The main reason was that the production cost was high, the product purity did not meet the requirements, and the technology was not qualified.
At present, there is no manufacturer producing leaf alcohol in China, and all products rely on imports

Method used

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Examples

Experimental program
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Embodiment

[0033] Step 1: Preparation of butyne-1

[0034] Add 200g of bromine into a 500ml three-necked flask, and pass through butene-1 in an ice-water bath until the color of the solution fades to obtain 1,2-dibromobutane, which is then distilled and purified for use.

[0035] In a 300ml three-neck flask with stirring and reflux condenser, add 100g of potassium hydroxide, heat to 130°C, slowly add 80g of 1,2-dibromobutane dropwise, and continuously produce butyne- 1 gas 15g, gas chromatography analysis content of more than 90%.

[0036] Step 2: Preparation of 3-hexyn-1-ol

[0037] Add 500ml of anhydrous tetrahydrofuran to a 1000ml three-neck flask with a stirring and reflux condenser connected to a nitrogen protection device, add 36g of magnesium chips and 5g of iodine under constant stirring, reflux, and nitrogen protection, and then slowly add bromoethane , to obtain ethylmagnesium bromide. Next, 80 g of butyne-1 prepared in step 1 was passed through at normal temperature and nor...

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Abstract

The present invention relates to high grade perfume leaf alcohol named chemically as cis-3-hexenol and with molecular expression of C6H12O and molecular weight 100-16. Specifically, the present invention synthesizes cis-3-hexenol with butene-1 as material and through bromination, dedebromination under alkaline condition to obtain 1-butine, exchange reaction of 1-butine and alkane bromide under the action of Grignard reagent, reaction with ethylene epoxide, hydrolysis to obtain 3-hexyne-1-alcohol, and final imperfect hydrogenation at normal temperature and normal pressure. The present invention has product purity over 99 %, and has easy-to-obtain material and low cost.

Description

technical field [0001] The present invention relates to advanced essence fragrance leaf alcohol (Leaf Alcohol) [scientific name: cis-3-hexene-1-alcohol (Cis-3-Hexenol); Molecular formula C 6 h 12 O; Molecular weight 100.16] synthetic method, be specifically the method for raw material synthesis leaf alcohol with butene. Background technique [0002] Leaf Alcohol [scientific name: cis-3-hexenol (Cis-3-Hexenol); C 6 h 12 ;Molecular weight 100.16;], in pure and high concentration, it has an ether-like green leafy aroma, and when diluted, it is a freshly cut green grass aroma, with a fresh and relaxing natural effect, such as the feeling of being in the summer wilderness; d 20 : 0.846; bp: 156~157℃; flash point: 44℃, solubility: slightly soluble in water, soluble in ethanol, organic esters, ketones, alcohols and glycols. [0003] Leaf alcohol occupies a special position in synthetic fragrances, and its importance lies in its unique natural fragrance. Leaf alcohol and its de...

Claims

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Application Information

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IPC IPC(8): C07C33/025C07C29/00C07C29/36
Inventor 闫圣刚范正林陶寅松徐长安李旋丛卫军张涛高绪国
Owner 大连圣迈化学有限公司
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