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Method for preparing alpha-angelica lactone from acetylpropionic acid

A technology of levulinic acid and angelica lactone, which is applied in chemical instruments and methods, molecular sieve catalysts, organic chemistry, etc., can solve the problems of side reactions and high reaction temperature, and achieve the effect of improving selectivity and high purity

Active Publication Date: 2009-07-08
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Meng Guangyu of Shandong General Group (Shandong Food Fermentation, 2004, 135, 62-64.) and a U.S. patent (U.S.Pat.No.2,809,203, issued Oct.8, 1957.) both reported a non-catalytic preparation The method of α-angelica lactone, but the reaction temperature is high, there are side reactions, and the α-angelica lactone is partially isomerized to generate β-angelica lactone, and the product contains about 10% β-angelica lactone

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Weigh 46g of levulinic acid into a flask, add 1ml of phosphoric acid, heat up to 150°C under stirring, control the vacuum of the reaction system to be 150mmHg, and the levulinic acid and α-angelica lactone in the gas phase of the reaction system pass through θ The ring packing column is separated, the levulinic acid is refluxed into the reaction system, the α-angelica lactone vapor slips out from the distillation head, the temperature at the distillation head is controlled at 87-90°C, and the condensed liquid is collected.

[0022] (2) The liquid product collected is vacuum distilled under 60mmHg pressure, and the cut of 75~78 ℃ is collected to obtain 35g α-angelica lactone with a purity of 90%.

Embodiment 2

[0024] (1) Weigh 45g of levulinic acid and put it into a flask, add 3ml of sulfuric acid, heat up to 150°C under stirring, control the vacuum of the reaction system to be 140mmHg, and the levulinic acid and α-angelica lactone in the gas phase of the reaction system are passed through the The West Ring packing column is separated, levulinic acid is refluxed into the reaction system, α-angelica lactone vapor slips out from the distillation head, the temperature at the distillation head is controlled at 84-87°C, and the condensed liquid is collected.

[0025] (2) The collected liquid product was vacuum distilled under a pressure of 50 mmHg, and the cuts at 70 to 74° C. were collected to obtain 34.5 g of α-angelica lactone with a purity of 94%.

Embodiment 3

[0027] (1) Weigh 48g of levulinic acid and put it into a flask, add 5ml of hydrochloric acid, heat up to 140°C under stirring, control the vacuum of the reaction system to be 120mmHg, and the levulinic acid and α-angelica lactone in the gas phase of the reaction system are passed through the The West Ring packing column is separated, the levulinic acid is refluxed into the reaction system, the α-angelica lactone vapor slips out from the distillation head, the temperature at the distillation head is controlled at 80-83°C, and the condensed liquid is collected.

[0028] (2) The collected liquid product was vacuum distilled under a pressure of 50 mmHg, and the cuts at 70 to 74° C. were collected to obtain 37 g of α-angelica lactone with a purity of 92%.

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PUM

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Abstract

The invention provides a method for preparing alpha-angelica lactone by levulinate. The method comprises the following steps: an inorganic liquid acid or a solid acid catalyst which is 1 to 10 weight percent of the levulinate is added into the levulinate; the levulinate and the alpha-angelica lactone in a gaseous phase of a reaction system are separated by rectifying at a temperature of between 100 and 150 DEG C with vacuum degree of between 20 and 150mmHg; the levulinate returns to the reaction system; the alpha-angelica lactone is condensed at a temperature of between 60 and 90 DEG C; and the product is obtained through separating and rectifying. The method has the advantages of high selectivity, high purity, and applicability of serialized industrial production.

Description

technical field [0001] The invention belongs to a method for preparing α-angelica lactone, in particular to a method for preparing α-angelica lactone from levulinic acid. Background technique [0002] α-Angelica lactone (C 5 h 6 o 2 , Mw=98.10), the chemical name is 4-hydroxyl-3-pentenolide or 5-methyl-2(3H)-furanone, which has a pleasant sweet smell and grassy fragrance similar to tobacco aroma, and is Colorless or light yellow oily liquid, when the temperature is lower than 18℃, it becomes needle crystal. It can emit a harmonious aroma with cigarette incense, caramel aroma, chocolate aroma, etc. It is an important food flavor, and it is also one of the main aroma components in tobacco. It has been widely used in the food and tobacco industries. But at present in our country, this product mainly relies on imports, which has seriously affected the popularization and utilization of this product in the food and cigarette industries. [0003] There are mainly two methods f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/58B01J27/02B01J27/16B01J27/10B01J21/04B01J21/06B01J29/40
Inventor 侯相林陈铁牛邓天昇
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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