Method for synthesizing gamma-lactone and perfume processing method thereof

A synthesis method and technology of lactone, which is applied in the field of synthesis of γ-lactone, can solve the problems of affecting quality, complicated reaction and high cost

Active Publication Date: 2010-06-16
北京北达正元科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, the above method is carried out in an autoclave, resulting in complex reactions and high costs
[0008] Moreover, the gamma-lactone that above-mentioned method obtains has obvious plastic smell or sour taste, has influenced its quality

Method used

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  • Method for synthesizing gamma-lactone and perfume processing method thereof
  • Method for synthesizing gamma-lactone and perfume processing method thereof
  • Method for synthesizing gamma-lactone and perfume processing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: Synthesis of γ-propyl-γ-butyrolactone

[0033] In the reactor equipped with stirrer, condenser, thermometer and dropping device, add 222 grams (3.0 moles) of butanol, heat it to reflux, and add dropwise over 7 hours while stirring. The mixed solution of 74 grams (1.0 mole) of butanol, 86 g (1.0 mole) of methyl acrylate and 58 grams (0.3 mole) of tert-butyl peroxybenzoate, continue to react at this temperature for 3 hours after completion of the dropwise addition, then cool down To room temperature, recover excess butanol, and then carry out rectification under reduced pressure to obtain 75.5 g of γ-propyl-γ-butyrolactone, and the calculated yield is 59.0%.

Embodiment 2

[0034] Embodiment 2: Synthesis of γ-hexyl-γ-butyrolactone

[0035] In a reactor equipped with a stirrer, a condenser, a thermometer and a dropping device, add 348 grams (3.0 moles) of heptanol, heat it to 160°C, and drop it over 7 hours while stirring. Add the mixed solution of 116 grams (1.0 moles) of heptanol, 86 g (1.0 moles) of methyl acrylate and 39 grams (0.2 moles) of tert-butyl peroxybenzoate, continue to react at this temperature for 3 hours after completion of the dropwise addition, and then Cool down to room temperature, recover excess heptanol, and then carry out rectification under reduced pressure to obtain 153 g of γ-hexyl-γ-butyrolactone, and the calculated yield is 90.0%.

Embodiment 3

[0036] Embodiment 3: Synthesis of γ-pentyl-γ-butyrolactone

[0037] In a reactor equipped with a stirrer, a condenser, a thermometer and a dropping device, add 306 grams (3.0 moles) of hexanol, heat it to 150°C, and drop it over 7 hours while stirring. Add the mixed solution of 102 grams (1.0 mole) of hexanol, 72 g (1.0 mole) of acrylic acid and 39 grams (0.2 mole) of tert-butyl peroxybenzoate, continue to react at this temperature for 3 hours after the dropwise addition, then cool down to At room temperature, excess heptanol was recovered, and then rectified under reduced pressure to obtain 138.8 g of γ-pentyl-γ-butyrolactone, and the calculated yield was 89.0%.

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PUM

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Abstract

The invention provides a method for synthesizing gamma-lactone and a perfume processing method thereof. In the synthesizing method, the alcohol shown as the following general formula (2) and 2-olefine acid or ester thereof shown as the following general formula (3) react by using t-butylperbenzoate at normal pressure to obtain gamma-lactone shown as the general formula (1). In the general formula (1), the general formula (2) and the general formula (3), R1 represents the alkyl of C3 to C10; R2 represents a hydrogen atom, methyl or ethyl; R3 represents a hydrogen atom or the alkyl of C1 to C6; R4 and R5 can be same or different and respectively represent a hydrogen atom or methyl; and R6 represents H, methyl or ethyl. The gamma-lactone can be obtained with high yield and low cost at normal pressure according to the synthesizing method. The invention also provides a perfume processing method. The gamma-lactone is processed by one of carbonate, bicarbonate, active carbon, a molecular sieve, sodium hydroxide, potassium hydroxide and kieselguhr to obtain the high-quality gamma-lactone from which plastic odor and sour odor are removed.

Description

technical field [0001] The invention relates to a synthesis method of gamma-lactone and a fragrance treatment method thereof. Background technique [0002] At present, regarding the synthetic method of γ-lactone shown in following general formula (1), known for example with acrylate and primary alcohol, in the presence of di-tert-butyl peroxide and phosphate and / or sulfate Carry out heating reaction to manufacture the method for gamma-alkyl-gamma-butyrolactone (referring to Japanese Patent Laid-Open No. 51-95058 communique); A method of producing γ-alkyl-γ-butyrolactone by reacting in the presence of the compound (see JP-A-55-133371). [0003] [0004] In general formula (1), R 1 means C 3 ~C 10 the alkyl group; R 2 Represents a hydrogen atom, methyl or ethyl; R 3 stands for hydrogen atom or C 1 ~C 6 the alkyl group; R 4 and R 5 Can be the same or different, each represents a hydrogen atom or a methyl group; R 6 Indicates H, methyl or ethyl. [0005] But above...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33
Inventor 王川卫小广吴文德邵永久
Owner 北京北达正元科技有限公司
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