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Method for synthesizing anisole by utilizing sodium methyl sulfate

A technology of sodium methyl sulfate and anisole, which is applied in chemical instruments and methods, alkali metal sulfite/sulfite, ether preparation and other directions, can solve problems such as not being industrialized, and achieve high conversion rate, high yield effect

Inactive Publication Date: 2018-04-06
SHAANXI HUANKE BIOLOGICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

etc., but due to problems in the treatment of three wastes and product quality, none of them have been industrialized

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The method utilizing sodium methylsulfate to synthesize anisole may further comprise the steps:

[0023] (1) Dissolve phenol in a sodium hydroxide solution with a mass concentration of 20%, wherein the molar ratio of phenol to sodium hydroxide is 1:2 to obtain a sodium phenoxide solution;

[0024] (2) According to the addition ratio of sodium phenate solution and sodium methyl sulfate: 100mL: 5.9g, add sodium methyl sulfate to the sodium phenate solution, reflux reaction at 110°C for 6h, then cool down to 40°C, add sulfuric acid dropwise to adjust The pH is 5, let it stand for 14 hours, separate the upper and lower layers, the upper layer is anisole, and the lower layer is an inorganic phase;

[0025] (3) washing the anisole obtained in step (2) twice with a sodium hydroxide solution with a mass concentration of 10%, and then drying with anhydrous sodium sulfate;

[0026] (4) Microwave the product of step (3) for 30 minutes under the condition of power of 200W, then ul...

Embodiment 2

[0029] The method utilizing sodium methylsulfate to synthesize anisole may further comprise the steps:

[0030] (1) Dissolving phenol in a sodium hydroxide solution with a mass concentration of 20%, wherein the molar ratio of phenol to sodium hydroxide is 1:1 to obtain a sodium phenoxide solution;

[0031] (2) According to the addition ratio of sodium phenate solution and sodium methyl sulfate is 100mL: 5.9g, add sodium methyl sulfate to the sodium phenate solution, reflux at 100°C for 6h, then cool down to 40°C, add sulfuric acid dropwise to adjust The pH is 5, let it stand for 10 hours, separate the upper and lower layers, the upper layer is anisole, and the lower layer is an inorganic phase;

[0032] (3) washing the anisole obtained in step (2) twice with a sodium hydroxide solution with a mass concentration of 10%, and then drying with anhydrous sodium sulfate;

[0033] (4) Microwave the product of step (3) for 30 minutes under the condition of power of 100W, then ultraso...

Embodiment 3

[0036] The method utilizing sodium methylsulfate to synthesize anisole may further comprise the steps:

[0037] (1) Dissolving phenol in a sodium hydroxide solution with a mass concentration of 20%, wherein the molar ratio of phenol to sodium hydroxide is 1:1.2 to obtain a sodium phenoxide solution;

[0038] (2) According to the addition ratio of sodium phenate solution and sodium methyl sulfate is 100mL: 5.9g, add sodium methyl sulfate to sodium phenate solution, reflux reaction at 105°C for 6h, then cool down to 40°C, add sulfuric acid dropwise to adjust The pH is 5, let it stand for 12 hours, separate the upper and lower layers, the upper layer is anisole, and the lower layer is an inorganic phase;

[0039] (3) washing the anisole obtained in step (2) twice with a sodium hydroxide solution with a mass concentration of 10%, and then drying with anhydrous sodium sulfate;

[0040] (4) Microwave the product of step (3) for 30 minutes at a power of 100 W, then ultrasonically di...

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PUM

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Abstract

The invention discloses a method for synthesizing anisole by using sodium methyl sulfate, which comprises the following steps: (1) dissolving phenol in sodium hydroxide solution to obtain a sodium phenoxide solution; (2) adding methyl to the sodium phenoxide solution Sodium sulfate, reflux reaction at 100-110°C for 6h, then lower the temperature to 40°C, add sulfuric acid dropwise to adjust the pH to 5, let stand for 10-14h, separate layers, separate the upper and lower layers, the upper layer is anisole, and the lower layer is Inorganic phase; (3) Wash the anisole obtained in step (2) twice with sodium hydroxide solution, and then dry with anhydrous sodium sulfate; (4) Microwave the product of step (3) for 30 minutes, and then ultrasonically disperse 20‑40min, naturally cooled to room temperature; (5) distilled at 110‑130°C for 50‑80min to obtain anisole. In the method provided by the invention, the conversion rate of phenol is high and the yield of anisole is high.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for synthesizing anisole by using sodium methyl sulfate. Background technique [0002] Anisole, also known as anisole, is an important organic synthesis intermediate, which can be used to synthesize pesticides, dyes and spices. It can be used to prepare many floral flavors, especially gardenia, lilac, and sunflower flavors. It can also be used as Antioxidant for oil and beer, plastic stabilizer, UV stabilizer for synthetic ethylene polymer, and an excellent solvent. [0003] Anisole can be synthesized by sodium phenate and methyl chloride, bromobenzene and methanol, methanol and phenol under strong acid catalyst system or zeolite catalyst. At present, anisole is usually synthesized by dimethyl sulfate and phenol in industry. Dimethyl sulfate is a highly toxic substance, and if used carelessly, it will cause great harm to the human body and the env...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/16C07C41/42C07C43/205C07C37/66C07C39/235C01D5/00
CPCC07C41/16C01D5/00C07C37/66C07C41/42C07C43/205C07C39/235
Inventor 郝青
Owner SHAANXI HUANKE BIOLOGICAL TECH CO LTD
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