Method for synthesizing gamma lactone

A synthesis method and lactone technology, applied in the direction of organic chemistry, can solve the problems of reduced reaction efficiency, complicated reaction device, and influence on product purity, and achieve the effect of improving product yield

Inactive Publication Date: 2011-02-16
ANHUI HYEA AROMAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Many domestic research institutions have conducted research on this process, and found that the optimum temperature for the addition reaction of acrylic acid or acrylate and alcohol is between 165 and 185°C, which is affected by the boiling point of the starting material. When the system reaches such a temperature, it can only be pressurized or a large amount of high-boiling-point s

Method used

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  • Method for synthesizing gamma lactone
  • Method for synthesizing gamma lactone

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0015] Example 1 (Gammaundecanolide)

[0016] a ingredients

[0017] 172g (2.0mol) of methyl acrylate; 2000g (15.4mol) of octanol; 30g (0.2mol) of di-tert-butyl peroxide; 1.7g of SL-90 polymerization inhibitor was added to stirring pot 1, the temperature dropped to -5℃ , Stir for 10 minutes;

[0018] b reaction

[0019] The above ingredients are continuously fed into the 1L autoclave 2 through the pump 3 through the feeding device, and the flow rate is controlled to 160g / hour; the nitrogen is pressurized to 0.25Mpa, and the temperature is raised and controlled at 190℃; after 5 hours, the top of the fractionation tower 5 starts to separate the sub Product methanol, tert-butanol and other by-products; recover unreacted octanol at the bottom of the tower to the reflux tank 8; continuously produce reaction products from the pump 4, and control the flow rate of the produced reactants to maintain the liquid level of the reactor; after 10 hours, react The content of the crude product reach...

Example Embodiment

[0021] Example 2 (Pro-nonanolactone)

[0022] a ingredients

[0023] 200g of methyl acrylate; 1900g of hexanol; 40g of di-tert-butyl peroxide; 1.7g of SL-90 polymerization inhibitor was added to stirring pot 1, the temperature was lowered to -5°C, and the mixture was stirred for 10 minutes;

[0024] b reaction

[0025] The above ingredients are continuously fed into the 1L autoclave 2 through the pump 3 through the feeding device, and the flow rate is controlled to 160g / hour; the nitrogen is pressurized to 0.25Mpa, and the temperature is raised and controlled at 190℃; after 5 hours, the top of the fractionation tower 5 starts to separate the sub Product methanol, tert-butanol and other by-products; recover unreacted hexanol at the bottom of the tower to the reflux tank 8; continuously produce reaction products from the pump 4, and control the flow rate of the produced reactants to maintain the liquid level of the reactor; after 10 hours, react The content of the crude product reaches...

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Abstract

The invention discloses a method for synthesizing gamma lactone. The method comprises the following steps of: putting acrylic acid or acrylic ester as well as alcohol and a ditertiary butyl peroxide or benzoyl peroxide into a stirring pot by a molar ratio of 1:(3-30); uniformly mixing at -20-30 DEG C; adding accessories to a kettle type reactor from a fractionating column which is filled with a cy700 stainless steel ripple filler and has 5-30 theoretical plates; controlling the flow rate to 50-200g/hour and the reaction temperature between 165 DEG C and 280 DEG C and pressurizing nitrogen to 0.05-1.25MPa; after 5 hours, fractionating out tertiary butanol and low-carbon ester which are byproducts under normal pressure through the fractionating column, and recovering unacted alcohol; after 10 hours, under vacuum pressure of 133-1,000Pa, extracting a crude reaction product from the reactor; and fractionating the crude product in a rectifying column to obtain a product. The method effectively improves the product yield, and the product quality conforms to the requirement on food blending.

Description

1. Technical field [0001] The invention relates to a method for synthesizing gamma lactone. 2. Background technology [0002] Gamma-lactone is a series of synthetic fragrances, including ga-caprolactone, ga-enantholactone, ga-caprolactone, ga-nonanolide, ga-decalactone, ga-undecalactone, ga-deca Dilactone. In the early days, heptanal and malonic acid were condensed and decarboxylated to synthesize gamma-nonanolide, and undecylenic acid sulfuric acid was used to synthesize gamma-undecalactone, both of which were replaced due to high cost. Japanese Patent No. 04-054177 describes the synthesis method of gamma-lactone series products. Using di-tert-butyl peroxide as a catalyst, acrylic acid or methyl acrylate and alcohol undergo free radical addition reaction in a high-pressure reactor. One-step synthesis Gamma lactone, changing different raw material alcohols to obtain lactone series products. Many domestic research institutions have conducted research on this process, and f...

Claims

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Application Information

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IPC IPC(8): C07D307/33
Inventor 范一义
Owner ANHUI HYEA AROMAS
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