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Preparation method of 4-methylanisole

A technology for p-methyl anisole and p-cresol is applied in the field of preparation of fine chemical intermediate p-methyl anisole, and can solve the problems of high cost, high waste water, low utilization rate of dimethyl sulfate, and the like, Achieve the effect of high utilization rate and zero discharge of wastewater

Inactive Publication Date: 2019-07-26
XINCHANG COUNTY TAIRU TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] 1. The utilization rate of dimethyl sulfate is low and the cost is high;
[0014] 2. There is a lot of waste water and it is difficult to deal with it

Method used

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  • Preparation method of 4-methylanisole
  • Preparation method of 4-methylanisole
  • Preparation method of 4-methylanisole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Neutralization reaction:

[0043] The p-cresol dropped into in the 1000ml four-neck flask with thermometer, stirring paddle, nitrogen pipe, recovery condenser: 100.0g (content: 99.1%, 0.9176mol), dehydrated alcohol: 600ml, open nitrogen protection, Set nitrogen flow rate: 0.5l / min. The outer wall of the four-necked flask is cooled with cooling water, and the inner temperature is controlled not to exceed 35° C. Slowly add sodium hydroxide: 37.5 g (0.9375 mol) into the four-necked flask from the thermometer mouth (pull out the thermometer). After feeding, the reaction was stirred for 1.0 hour. After the reaction is completed, the outer wall of the four-neck flask is heated with 85-90°C hot water, and the ethanol is continuously distilled out under the protection of nitrogen. In the later stage of distillation, the outflow velocity of ethanol will become smaller and smaller. When the outflow of ethanol is very small, vacuum recovery is carried out, and the vacuum degree...

Embodiment 2

[0053] Neutralization reaction:

[0054] 100.0 g (content: 99.1%, 0.9176 mol) of p-cresol dropped into a four-necked flask with a thermometer, stirring paddle, nitrogen pipe, and recovery condenser in 1000 ml, anhydrous n-butanol: 600 ml, nitrogen Protection, set nitrogen flow rate: 0.5l / min. The outer wall of the four-necked flask is cooled with cooling water, and the inner temperature is controlled not to exceed 35° C. Slowly add sodium hydroxide: 37.5 g (0.9375 mol) into the four-necked flask from the thermometer mouth (pull out the thermometer). After feeding, the reaction was stirred for 1.0 hour. After the reaction is completed, the outer wall of the four-necked flask is heated with an electric heating mantle, and the vacuum recovery is carried out under the protection of nitrogen, and the vacuum degree is gradually increased. Finally, the internal temperature is controlled to be less than 100°C, and the vacuum degree is greater than -0.08MPa to recover n-butanol to dry...

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Abstract

The invention discloses a preparation method of 4-methylanisole. The method includes: using p-cresol and sodium hydroxide as the raw materials to prepare p-methylphenol sodium; allowing the p-methylphenol sodium and dimethyl sulfate to have methylation in a nonpolar solvent to prepare the 4-methylanisole and byproduct sodium methylsulfate; allowing the p-methylphenol sodium and the byproduct sodium methylsulfate to have reaction in a polar solvent to prepare the 4-methylanisole and sodium sulfate. The method has the advantages that the 4-methylanisole is prepared through the three-step reaction, the utilization rate of the dimethyl sulfate is increased, and wastewater zero discharge is achieved.

Description

technical field [0001] The invention relates to the field of fine organic chemical synthesis, in particular to a method for preparing a fine chemical intermediate p-methylanisole. Background technique [0002] p-methylanisole (p-methoxytoluene), English name: 4-Methylanisole. P-methylanisole is an important fine chemical intermediate, which is used to synthesize p-methoxybenzaldehyde in the fragrance industry. p-methoxybenzaldehyde is a kind of fragrance with high application value and can be used to synthesize many Acetal spices; used in the preparation of amoxicillin in the pharmaceutical industry; used in the preparation of functional polymer materials in the polymer industry; used in the preparation of metal brighteners in the electroplating industry; Pesticide additives, plant growth regulators, etc. [0003] The method for preparing p-methylanisole with p-cresol as raw material mainly contains following 3 kinds. 1. Methylation reaction of p-cresol and dimethyl sulfa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/16C07C43/205
CPCC07C37/66C07C41/16C07C39/235C07C43/205
Inventor 赵德英
Owner XINCHANG COUNTY TAIRU TECH CO LTD
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