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Synthetic method for organic synthesis intermediate octanal

A technology of organic synthesis and synthesis method, which is applied in the preparation of organic compounds and the synthesis of octanal, an intermediate of organic synthesis, can solve the problems of non-compliance with green energy saving, economical and environmental protection, complex synthesis process and high heat resistance requirements of equipment, and achieve Avoid the adverse effects of greater environmental pollution, increase the reaction yield, and reduce the heat resistance requirements of the equipment

Inactive Publication Date: 2018-07-03
CHENGDU QIANYE LONGHUA PETROLEUM ENG TECH CONSULTING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This synthesis method requires a high-temperature environment above 300°C, requires a lot of energy consumption, requires high heat resistance of the equipment, has a high loss rate of the equipment, and increases the production cost. The processing cost is also high, so this synthesis method does not meet the requirements of green energy saving, economy and environmental protection, and the whole synthesis process is relatively complicated, so it is necessary to propose a new synthesis method

Method used

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  • Synthetic method for organic synthesis intermediate octanal
  • Synthetic method for organic synthesis intermediate octanal
  • Synthetic method for organic synthesis intermediate octanal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] The synthetic method of organic synthesis intermediate octanal, comprises the steps:

[0013] A: Add 3mol 1-aminooctane and 1.2L anhydrous p-chlorotoluene solution into the reaction vessel, raise the solution temperature to 40°C, control the stirring speed at 170rpm, react for 90min, add 3mol tungsten disulfide powder, and continue the reaction for 2h;

[0014] B: Then add 3 mol of anhydrous isobutyl formate solution, reflux for 80 minutes, lower the temperature to 10°C, let stand for 1 hour, wash with anhydrous 1,3-dichloropropane solution 3 times, and anhydrous diisopropane solution 6 times , recrystallized in anhydrous m-xylene solution, and dehydrated with an activated alumina dehydrating agent to obtain 334.08 g of octanal, a yield of 87%.

Embodiment 2

[0016] The synthetic method of organic synthesis intermediate octanal, comprises the steps:

[0017] A: Add 3mol 1-aminooctane and 1.2L anhydrous p-chlorotoluene solution to the reaction vessel, raise the temperature of the solution to 45°C, control the stirring speed at 180rpm, react for 110min, add 3.6mol tungsten disulfide powder, and continue the reaction 2.8 h;

[0018] B: Then add 5mol anhydrous isobutyl formate solution, reflux for 90min, lower the temperature to 13°C, let it stand for 1.3h, wash with anhydrous 1,3-dichloropropane solution 4 times, and anhydrous diisopropane solution for 7 The second time, recrystallized in anhydrous m-xylene solution, and dehydrated with anhydrous potassium carbonate dehydrating agent to obtain 349.44 g of finished octanal, with a yield of 91%.

Embodiment 3

[0020] The synthetic method of organic synthesis intermediate octanal, comprises the steps:

[0021] A: Add 3mol 1-aminooctane and 1.2L anhydrous p-chlorotoluene solution into the reaction vessel, raise the temperature of the solution to 46°C, control the stirring speed to 210rpm, react for 120min, add 4mol tungsten disulfide powder, and continue the reaction for 3h;

[0022] B: Then add 6mol anhydrous isobutyl formate solution, reflux for 110min, lower the temperature to 15°C, let stand for 2h, wash with anhydrous 1,3-dichloropropane solution for 5 times, and anhydrous diisopropane solution for 8 times , recrystallized in anhydrous m-xylene solution, and dehydrated with an activated alumina dehydrating agent to obtain 360.96 g of octanal, a yield of 94%.

[0023] Table 1 Infrared analysis data

[0024]

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Abstract

The invention discloses a synthetic method for the organic synthesis intermediate octanal. The synthetic method comprises the following steps: adding 1-aminooctane and an anhydrous p-chorotoluene solution into a reaction vessel, raising a solution temperature, controlling a stirring speed, carrying out a reaction, adding tungsten disulfide powder and continuing the reaction; and then adding an anhydrous isobutyl formate solution, carrying out a refluxing reaction, lowering the temperature, carrying out standing, then carrying out washing with an anhydrous 1,3-dichloropropane solution a plurality of times, carrying out washing with an anhydrous diisopropane solution a plurality of times, then carrying out recrystallization in an anhydrous xylene solution and carrying out dehydration with adehydrating agent to obtain the finished octanal.

Description

technical field [0001] The invention relates to a method for preparing an organic compound, which belongs to the field of organic synthesis, in particular to a method for synthesizing an organic synthesis intermediate octanal. Background technique [0002] Octanal is an intermediate in organic synthesis, and is one of the components of rose top fragrance. It is also used in sweet orange blossom, bitter orange blossom, bergamot and citrus colognes. It can also be used in a small amount to imitate food flavors such as cream, chocolate, apricot, plum, grape, lemon, sweet orange, and cheese. Octanal has a strong fruity aroma, and it has a pleasant sweet orange aroma when it is very dilute. It is mainly used in the blending of citrus flavors. The dosage in beverages, ice cream, candy, bread, etc. is 1.4-4.4ppm. It can also be used as a fragrance for soap and detergent. Most of the existing synthetic methods use the mixture of octanoic acid vapor and excess formic acid vapor to ...

Claims

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Application Information

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IPC IPC(8): C07C45/51C07C47/02
CPCC07C45/516C07C47/02
Inventor 关艮安
Owner CHENGDU QIANYE LONGHUA PETROLEUM ENG TECH CONSULTING
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