CN102476981A

CN102476981A - Method for preparing 1,3,5-trimethoxybenzene

Info

Publication number: CN102476981A
Application number: CN 201010555746
Authority: CN
Inventors: 韩文彬; 王辰; 王木兰; 张克森
Original assignee: TIANJIN SANNONGJIN TECHNOLOGY Co Ltd
Current assignee: TIANJIN SANNONGJIN TECHNOLOGY Co Ltd
Priority date: 2010-11-23
Filing date: 2010-11-23
Publication date: 2012-05-30

Abstract

The present invention relates to a method for preparing 1,3,5-trimethoxybenzene. The method comprises allowing reaction of sodium and methanol to obtain a methanol solution of sodium methoxide, adding dimethylformamide, then adding cuprous iodide and 1,3,5-tribromobenzene, heating to 80-90 DEG C, refluxing and reacting under stirring for 2-3 h, filtering to obtain a filtrate, distilling the filtrate under a reduced pressure to remove methanol and dimethylformamide, distilling with steam to obtain a distillate, cooling the distillate, crystallizing, filtering, and drying to obtain the final product. The invention has low production cost. The prepared 1,3,5-trimethoxybenzene has high purity and yield up to above 80%.

Description

1,3, the preparation method of 5-trimethoxy-benzene

Technical field:

The invention belongs to a kind of compound method of fine-chemical intermediate, particularly a kind of 1,3, the preparation method of 5-trimethoxy-benzene.

Background technology:

1,3, the 5-trimethoxy-benzene is important organic synthesis intermediate, is mainly used in medical manufacturing field.1,3, the 5-trimethoxy-benzene is a kind of white crystalline powder, and is water insoluble.Preparation 1,3 at present, the method production cost of 5-trimethoxy-benzene is high, yield is generally less than 70%, and the total cost of the finished product is higher.

Summary of the invention:

The object of the invention just is to overcome the deficiency that exists in the above-mentioned prior art, and provides a kind of 1,3, the preparation method of 5-trimethoxy-benzene, and the production cost of this method is low, the yield of products obtained therefrom high.

As above design, technical scheme of the present invention is: a kind of 1,3, the preparation method of 5-trimethoxy-benzene; It is characterized in that: sodium Metal 99.5 and methanol mixed are made methanol solution of sodium methylate, add N then, again with Cu2I2 and 1,3; The 5-tribromo-benzene adds, and is heated to 80-90 degree centigrade, and stirring and refluxing reaction 2-3 hour is filtered; Filtrate decompression steams methyl alcohol and N, has steamed the back and has used steam distillation, gained distillate crystallisation by cooling after-filtration, drying; Promptly get 1,3, the 5-trimethoxy-benzene.

Above-mentioned 1,3, the preparation method of 5-tribromo-benzene is characterized in that: ethanol with 95% and benzene add 2,4,6-tribromo-benzene heating for dissolving after mixing again; In 1-2 hour time, progressively add the vitriol oil again, stir, add the back holding temperature at 50-60 degree centigrade; Add NaNO then in batches ₂Boil insulation reaction 2-3 hour; Last cooling crystallization, filtration, water is washed till neutrality, is drying to obtain solid 1,3, the 5-tribromo-benzene.

Production cost of the present invention is low, gained 1,3, and the purity height of 5-trimethoxy-benzene, yield are up to more than 80%.

Embodiment:

A kind of 1,3, the preparation method of 5-trimethoxy-benzene, carry out according to the following step:

1, after being mixed, 95% ethanol and benzene adds 2,4 again, 6-tribromo-benzene heating for dissolving; In 1-2 hour time, progressively add the vitriol oil again, stir, add the back holding temperature at 50-60 degree centigrade; Add NaNO then in batches ₂Boil insulation reaction 2-3 hour; Last cooling crystallization, filtration, water is washed till neutrality, is drying to obtain solid 1,3, the 5-tribromo-benzene.

2,10g sodium Metal 99.5 and 80ml methanol mixed are made methanol solution of sodium methylate, add the 80ml N then, again with 2gCu2I2 and 20g1,3; The 5-tribromo-benzene adds, and is heated to 90 degrees centigrade, and stirring and refluxing reaction 3 hours is filtered; Filtrate decompression steams methyl alcohol and N, has steamed the back and has used steam distillation, gained distillate crystallisation by cooling after-filtration, drying; Promptly get 1,3, the 5-trimethoxy-benzene.

Claims

1. one kind 3, the preparation method of 5-trimethoxy-benzene is characterized in that: sodium Metal 99.5 and methanol mixed are made methanol solution of sodium methylate, add N then; With Cu2I2 and 1,3, the 5-tribromo-benzene adds, and is heated to 80-90 degree centigrade again; Stirring and refluxing reaction 2-3 hour is filtered, and filtrate decompression steams methyl alcohol and N, has steamed the back and has used steam distillation; Gained distillate crystallisation by cooling after-filtration, drying promptly get 1,3, the 5-trimethoxy-benzene.

2. according to claim 11,3, the preparation method of 5-trimethoxy-benzene is characterized in that: above-mentioned 1,3, the preparation method of 5-tribromo-benzene is characterized in that: ethanol with 95% and benzene add 2,4,6-tribromo-benzene heating for dissolving after mixing again; In 1-2 hour time, progressively add the vitriol oil again, stir, add the back holding temperature at 50-60 degree centigrade; Add NaNO then in batches ₂Boil insulation reaction 2-3 hour; Last cooling crystallization, filtration, water is washed till neutrality, is drying to obtain solid 1,3, the 5-tribromo-benzene.