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Preparation method of anisic aldehyde

A technology of anisaldehyde and temperature control, which is applied in the field of spices and flavors chemical industry, can solve the problems of a large amount of phosphorus-containing wastewater, and achieve the effect of easy industrial production and easy control

Active Publication Date: 2015-01-21
SUQIAN COSMOS CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, using POCl 3 Carrying out V's formylation reaction with N-methylformanilide and anisole is also one of the methods for preparing anisaldehyde, but this method will bring a large amount of phosphorus-containing wastewater

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] In a 500 ml glass reactor, 44.11 g of DMF and 3.16 g of pyridine were added while maintaining the temperature at 0-10°C. Then slowly add 59.35g triphosgene dissolved in 300g chloroform within 6h. When all the triphosgene is added, keep warm for 1h.

[0042] Add 75.2 g of aluminum trichloride to the above reaction solution in batches within 0.5 h, and keep the temperature at 20-30°C when adding aluminum trichloride. When all the aluminum trichloride is added, keep warm for 0.5h.

[0043] Then the chloroform in the above reaction system was distilled off until the kettle temperature reached 80°C. And gradually added 52.5 g of anisole within 3h. After the addition of anisole, the temperature was maintained at 80-85° C. for 6 hours while stirring.

[0044] After the reaction, the reaction solution was hydrolyzed with an aqueous solution of sodium hydroxide. After water separation, washing, and extraction, the solvent is removed to obtain the crude anisaldehyde, which i...

Embodiment 2

[0046] In a 500 ml glass reactor, 44.11 g of DMF and 4.26 g of pyridine were added while maintaining the temperature at 0-5°C. Then slowly add 61.47g triphosgene dissolved in 300g chloroform within 4h. When all the triphosgene is added, keep warm for 0.2h.

[0047] Add 75.2 g of aluminum trichloride to the above reaction solution in batches within 0.5 h, and keep the temperature at 20-30°C when adding aluminum trichloride. When all the aluminum trichloride is added, keep warm for 0.5h.

[0048] Then the chloroform in the above reaction system was distilled off until the kettle temperature reached 60°C. And gradually added 52.5 g of anisole within 2h. After the anisole was added, the temperature was maintained at 80-85° C. for 7 hours while stirring.

[0049] After the reaction, the reaction solution was hydrolyzed with an aqueous solution of sodium hydroxide. After water separation, washing and extraction, the solvent is removed to obtain the crude product of anisaldehyde...

Embodiment 3

[0051] In a 500 ml glass reactor, 44.11 g of DMF and 3.16 g of pyridine were added while maintaining the temperature at 0-5°C. Then slowly add 59.35g triphosgene dissolved in 300g chloroform within 7h. When all the triphosgene is added, keep warm for 0.5h.

[0052] Add 80 grams of aluminum trichloride to the above reaction solution in batches within 0.3 hours, and keep the temperature at 30-40°C when adding aluminum trichloride. When all the aluminum trichloride is added, keep warm for 0.5h.

[0053] Then the chloroform in the above reaction system was distilled off until the kettle temperature reached 80°C. And gradually added 53.5 g of anisole within 3h. After the addition of anisole, the temperature was kept at 80-85° C. for 10 hours while stirring.

[0054] After the reaction, the reaction solution was hydrolyzed with an aqueous solution of sodium hydroxide. After water separation, washing and extraction, the solvent is removed to obtain the crude product of anisaldeh...

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Abstract

The invention discloses a preparation method of anisic aldehyde. The preparation method comprises the following steps: 1, firstly adding N,N-dimethyl formamide and pyridine in a reaction kettle, then at a low temperature, dropping triphosgene dissolved by chloroform and carrying out a reaction, after dropping of triphosgene is finished, carrying out heat preservation, and continuing the reaction for 0.2-1 h; 2, keeping the low temperature, adding aluminum trichloride into the reaction liquid in batches, and after completing addition of aluminum trichloride, carrying out heat preservation for 0.2-1 h; 3, steaming out chloroform in the kettle, making the kettle temperature reach 60-100 DEG C, and slowly dropping anisole with keeping the temperature; 4, after completing dropping of anisole, continuing to heat and stir for 6-10 h at the temperature of 60-100 DEG C; and 5, after the reaction is finished, quenching the reaction liquid with a liquid caustic soda solution, washing, extracting, desolventizing, and rectifying to obtain the final product anisic aldehyde. The method has the characteristics of simpleness, easy control and industrialized production; and the produced anisic aldehyde is safe and stable, and the production efficiency is improved.

Description

technical field [0001] The invention relates to a method for preparing an organic intermediate, in particular to a method for preparing anisaldehyde, and belongs to the technical field of flavor and essence chemical industry. Background technique [0002] Anisic aldehyde (p-Anisaldehyde; Anisic aldehyde) pure product is a colorless or light yellow liquid with a strong hawthorn flower aroma, long-lasting aroma, and strong antioxidant properties. Anisaldehyde is the raw material for the synthesis of anisyl alcohol and its esters, anisic acid and its esters, and anisonitrile, and is also an important synthetic spice, widely used in the deployment of daily chemical flavors and food flavors. It can be used as the main fragrance in hawthorn flower, sunflower and lilac essence; it can be used as fragrance agent in lily of the valley essence; it can be used as modifier in osmanthus essence, and it can also be used in daily essence and food essence. This product is an edible spice t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/575C07C45/00C07C251/30C07C249/02
CPCC07C45/00C07C249/02C07C47/575C07C251/30
Inventor 杨正浩高翔周旭明杨东生
Owner SUQIAN COSMOS CHEM
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