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A kind of preparation method of m-fluoroanisole

A technology for m-fluoroanisole and m-difluorobenzene is applied in the field of preparation of m-fluoroanisole, can solve the problems of many steps, high industrialization cost, expensive process raw materials and the like, achieves less steps, reduced raw material cost, The effect of easy availability of raw materials

Active Publication Date: 2017-06-13
郓城县世炬商贸有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The raw materials of this process are relatively expensive, the steps are relatively many, and the industrialization cost is relatively high

Method used

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  • A kind of preparation method of m-fluoroanisole
  • A kind of preparation method of m-fluoroanisole
  • A kind of preparation method of m-fluoroanisole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Put 150kg of methanol into a 1000-liter carbon steel reactor, add 100kg of potassium hydroxide in four batches at a temperature of 20°C, and add 100kg of potassium hydroxide at a time interval of 20 minutes for each batch. DMSO (dimethyl sulfoxide) 180kg and cuprous chloride 4kg, heat up to 70°C, add m-difluorobenzene 160kg dropwise, the rate of addition is enough to maintain the reflux of the system, after dropping, keep warm at 80-90°C for 14 Hour. After heat preservation, add water and steam distillation to obtain a crude product, which is rectified by a rectification tower, and fractions at 101-102°C / 80mmHg are collected to obtain m-fluoroanisole. The yield is 82%, and the content is >99.5%.

Embodiment 2

[0024] Put 150kg of methanol into a 1000-liter carbon steel reaction kettle, add 105kg of potassium hydroxide in four batches at a temperature of 30°C, and add 105kg of potassium hydroxide in four batches, and the time interval between each batch is 20 minutes. (Dimethyl sulfoxide) 200kg and cuprous chloride 4kg, heat up to 75°C, add m-difluorobenzene 160kg dropwise, the rate of addition is enough to maintain the reflux of the system, after the drop is completed, keep the reaction at 85-90°C for 16 hours . After heat preservation, add water and steam distillation to obtain a crude product, which is rectified by a rectification tower, and fractions at 101-102°C / 80mmHg are collected to obtain m-fluoroanisole. The yield is 85%, and the content is >99.5%.

Embodiment 3

[0026] Put methanol 150kg into a 1000-liter carbon steel reaction kettle, add potassium hydroxide 100kg in four batches at a temperature of 40°C, and add 100kg of potassium hydroxide in four batches. The time interval between each batch of additions is 20 minutes. Dimethyl sulfoxide) 180kg and cuprous chloride 4kg, heat up to 80°C, add m-difluorobenzene 160kg dropwise, the rate of addition is enough to maintain the reflux of the system, after dropping, keep warm at 80-85°C for 15 hours. After heat preservation, add water and steam distillation to obtain a crude product, which is rectified by a rectification tower, and fractions at 101-102°C / 80mmHg are collected to obtain m-fluoroanisole. The yield is 83%, and the content is >99.5%.

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Abstract

The invention discloses a preparation method of m-fluoroanisole. The preparation method includes following steps: (1), adding methanol into a reaction kettle, heating to 20-60 DEG C, adding potassium hydroxide, and holding temperature; (2), continuing to add dimethyl sulfoxide and cuprous chloride into the reaction kettle, heating, and adding m-difluorobenzene for reaction for 14-18 h; (3), adding water into a reaction product, distilling to obtain a crude product, further rectifying to obtain m-fluoroanisole. The preparation method is easy-to-get and cheap in raw materials, few in steps, simple to operate and needless of high-pressure equipment, raw material cost and production cost are lowered greatly, product yield can reach higher than 80%, which is far higher than that of existing processes, and the preparation method is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of m-fluoroanisole. Background technique [0002] M-fluoroanisole is an important chemical intermediate, which is mainly used in the preparation of liquid crystals, pharmaceuticals, and pesticide intermediates. Its English name: 3-Fluoroanisole, molecular formula C 7 h 7 FO, CAS number is 456-49-5, structural formula is . [0003] At present, there are mainly two kinds of processes for preparing m-fluoroanisole from literature reports: one is to prepare m-fluoroanisole through Schiemann reaction by using m-aminoanisole, and its reaction equation is: [0004] [0005] The pyrolysis process of the synthesis method of this process is dangerous, the operating conditions are harsh, the industrialization is difficult, the total reaction yield is low, and the unit consumption is high. [0006] Another method for synthesizing m-fluoroan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/16C07C43/225
CPCC07C41/16C07C43/225
Inventor 陈维德刘拥贤
Owner 郓城县世炬商贸有限公司