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Method for synthesis of delta-undeca lactone

A synthesis method and lactone technology are applied in the field of synthesis of delta-undecalactone, can solve the problems of complicated delta-undecalactone process, low product yield and the like, achieve high product yield and purity, and simple process , the effect of less by-products

Inactive Publication Date: 2007-05-16
上海香料研究所
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  • Abstract
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  • Application Information

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Problems solved by technology

The δ-undecalactone obtained by the usual method is complicated and the product yield is low

Method used

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  • Method for synthesis of delta-undeca lactone

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Embodiment Construction

[0007] The implementation of the present invention will be further described below.

[0008] Add 140ml of formic acid and 56 grams of urea-peroxide adduct in a 500ml three-necked flask equipped with a stirrer, dropping funnel, and thermometer, and stir to dissolve. At room temperature, 28 g (0.17 mol) of 2-hexylcyclopentanone was added dropwise, and the dropwise addition was completed in about 1 hour. 168ml of water was added, the layers were stirred, the aqueous layer was extracted three times with 28ml of toluene, and the organic layers were combined. The toluene in the organic layer was removed by distillation under reduced pressure, and the temperature was controlled not to exceed 70°C. The residue was the crude product of δ-undecalactone with a purity of 85% and a yield of 96%. The crude product was distilled with a vacuum thin film distillation device, the temperature was controlled at 128° C., and the pressure was 1.4 kpa. The distilled product was δ-undecalactone with...

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Abstract

The invention discloses a synthesizing method of delta-hendelactone, which comprises the following steps: adopting aminic acid as solvent under indoor temperature; oxidizing 2-hexyl cyclopentanone and aquacare-peroxidate adduct to produce rough product at 25 Deg C for 1h; setting the aquacare-peroxidate adduct as oxidant; using vacuum film distillation method to purify to produce pure product.

Description

technical field [0001] The invention relates to a method for synthesizing δ-undecalactone. Background technique [0002] Delta-undecalactone has a sweet, fruity, milky, creamy, buttery, estery, waxy, coconut aroma and taste. The δ-undecalactone obtained by the usual method is complicated in technology and the product yield is low. Contents of the invention [0003] Aiming at the shortcomings of the prior art, the invention provides a method for synthesizing δ-undecalactone with higher yield. [0004] The synthetic method of δ-undecalactone of the present invention: under the condition of room temperature, take formic acid as solvent, use 2-hexylcyclopentanone and urea-peroxide adduct to obtain crude product through oxidation reaction, then use vacuum film The pure product was obtained by distillation. The urea-peroxide adduct is used as the oxidant, the reaction temperature is about 25°C, the reaction time is 1 hour, the solvent used in the reaction is formic acid, and ...

Claims

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Application Information

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IPC IPC(8): C07D309/16
Inventor 周治国
Owner 上海香料研究所