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Intermediate for synthesizing butene liquid crystal and synthetic method thereof

An intermediate and liquid crystal technology, applied in the preparation of sulfonate esters, organic chemistry, etc., can solve the problems of difficulty in choosing a good solvent to dissolve, the sulfonate ester is not easy to dissolve, and the raw material alcohol is difficult to convert, and the post-processing process is simple, fast and good. Decolorization, simple post-processing effects

Active Publication Date: 2009-04-15
HEBEI MAIERSTON ELECTRONICS MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are disadvantages in the current preparation process: 1. In this process, the raw material alcohol is difficult to completely convert, the crude product has low purity and cannot be directly used in the next step, and the yield is low
2. The post-treatment adopts the traditional process, which is cumbersome. After the reaction, the feed liquid needs to be washed many times, and the washing water phase often needs to use solvents to extract the product many times. The solvent dissolves, and a large amount of solvent is required for extraction, often due to insufficient extraction, and multiple washings and liquid separations cause product loss

Method used

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  • Intermediate for synthesizing butene liquid crystal and synthetic method thereof
  • Intermediate for synthesizing butene liquid crystal and synthetic method thereof
  • Intermediate for synthesizing butene liquid crystal and synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] [Example 1] preparation of

[0032] Will 8g (0.026mol), 5.3g (0.052mol) of triethylamine, and 60ml of THF were put into the bottle, and 5.9g (0.077mol) of methanesulfonyl chloride was added dropwise at 20°C, and the addition was completed in about 3 minutes. Reflux at 20°C for 10h. Then, evaporate 70% THF, add 50ml of water and stir for 1 hour, filter, and wash the filter cake once with 40ml of 50% ethanol. The product sulfonate was obtained, mp143°C, HPLC>97%, yield>97%.

Embodiment 2

[0033] [Example 2] preparation of

[0034] The specific operation is the same as in Example 1, the product mp>130°C, HPLC>97%, and yield>97%.

Embodiment 3

[0035] [Example 3] preparation of

[0036] The specific operation is the same as in Example 1, the product mp>150°C, HPLC>97%, and yield>97%.

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PUM

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Abstract

The invention relates to an intermediate for synthesizing butene liquid crystal and a synthesizing method thereof. The intermediate for synthesizing butene liquid crystal has a general formula structure as the right, which is shown in a right formula (I) or alkyl of C1-C7 or alkoxy of C1-C7; when in a right formula (II), X is H or F, Z is H or F, Y=F or alkyl of C1-C7 or alkoxy of C1-C7 or -OCHF2 or -OCF3 or -CF3 or CHF2; and n=0 or 1. The synthesizing method lies in that corresponded raw material alcohol is reacted with methyl sulfonic acid chloride in solvent with the presence of catalyst. The synthesizing method has a fast reaction without other side products, the post treatment process is simple and handy and the obtained product has high yield coefficient and purity.

Description

technical field [0001] The invention relates to a liquid crystal intermediate and a synthesis method thereof, in particular to an intermediate for synthesizing butene-based liquid crystals and a synthesis method thereof. Background technique [0002] In the LCD industry, Butene compounds are an important class of liquid crystal monomers, which are widely used in high-grade STN mixed crystals and TFT mixed crystals. In the patent JP2003095997, it is mentioned that a sulfonate ester is catalyzed by a copper salt to react with a Grignard reagent of a linear halide containing a double bond to form an alkene liquid crystal compound. In the patent JP, 61-83136, A mentions several other methods for synthesizing alkenes, but the synthesis route is long and the cost is high. At present, the mature routes for synthesizing such compounds are: [0003] [0004] Among them, the intermediate sulfonate is crucial to the synthesis of the final product butenes. The synthetic chemistr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/66C07C303/28
Inventor 仲锡军葛会军刘江宏梁建国
Owner HEBEI MAIERSTON ELECTRONICS MATERIAL
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