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Prepn process of 3-trifluoro methyl benzoate

A kind of technology of trifluoromethyl benzoate and trichloromethyl trifluoromethyl benzene, applied in the field of preparation of 3-trifluoromethyl benzoate

Inactive Publication Date: 2007-11-07
SHANGHAI CHEMSPEC CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no report yet to obtain the relatively easy and relatively cheap m-trichloromethyl trifluoromethyl benzene as raw material, directly prepare the method for 3-trifluoromethyl benzoic acid ester

Method used

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  • Prepn process of 3-trifluoro methyl benzoate
  • Prepn process of 3-trifluoro methyl benzoate
  • Prepn process of 3-trifluoro methyl benzoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Preparation of m-ditrichloromethylbenzene

[0074] After mixing 563 mole parts of m-ditrichloromethylbenzene and 1689 mole parts of m-xylene, the temperature inside the reactor was raised to 120°C, then the ultraviolet lamp was turned on, chlorine gas was introduced, and the temperature inside the reactor was kept at 120-140°C. The reaction was carried out for 30 hours. According to gas chromatography analysis, the content of m-dichloromethyltrichloromethylbenzene, an intermediate of the chlorination reaction, is lower than 0.5%. Measured by GC-MS method, the reaction product is m-ditrichloromethylbenzene.

[0075] Degassing under reduced pressure, distilling the reaction solution under reduced pressure, collecting fractions at 154-158°C / 10mmHg to obtain 2068 parts of m-ditrichloromethylbenzene, the yield of chlorination reaction was 89.3%, m-ditrichloromethyl The purity of benzene is 97.2%.

Embodiment 2-9

[0077] Preparation of m-ditrichloromethylbenzene

[0078] Proceed in the same manner as in Example 1, except that the reaction temperature, raw material ratio and reaction time are as shown in Table 1. Table 1 also shows the yield, the purity and the high boiler content of the obtained product of m-bistrichloromethylbenzene.

[0079] In addition, Example 8 uses 2% by weight of azobisisobutyronitrile (based on the weight of m-xylene) as an initiator instead of UV initiation.

Embodiment 9

[0080] Example 9 uses 2% by weight of benzoyl peroxide (based on the weight of m-xylene) as the initiator instead of UV initiation.

[0081] implement

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Abstract

The preparation process of 3-trifluoromethyl benzoate includes the following steps: adding water into m-trichloromethyl trifloromethyl benzene for hydrolysis in the presence of zinc-containing catalyst, and the subsequent adding hydroxyl compound ROH for esterification to produce 3-trifluoromethyl benzoate, where R is alkyl radical, aryl radical, alkaryl radical or aralkyl radical. The m-trichloromethyl trifloromethyl benzene is prepared through the fluoridation of meta-bis(trichloro methylbenzene) and hydrogen fluoride in the presence of catalyst; and meta-bis(trichloro methylbenzene) is prepared through the reaction of metaxylene and chlorine in meta-bis(trichloro methylbenzene) solvent under the action of initiator or photoinitiator.

Description

technical field [0001] The present invention relates to the preparation method of 3-trifluoromethyl benzoate. Background technique [0002] 3-trifluoromethylbenzoate (especially methyl 3-trifluoromethylbenzoate) is a very valuable intermediate, which has been widely used in the fields of pesticides, medicine and fine chemicals. [0003] In the prior art, the synthetic method of 3-trifluoromethylbenzoic acid methyl ester adopts to be raw material with 3-trifluoromethylbenzoic acid more, first obtains 3-trifluoromethylbenzoyl chloride with sulfur oxychloride reaction, Then react with methanol to obtain the product (see Polish Journal of Applied Chemistry, 47(3), 137-145; 2003). Another method is: esterify the 3-trifluoromethylbenzoic acid raw material in a methanol solution containing a catalytic amount of concentrated sulfuric acid to obtain the product. The first method will produce a large amount of waste gas sulfur dioxide and hydrogen chloride, which will pollute the en...

Claims

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Application Information

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IPC IPC(8): C07C69/78C07C67/00
Inventor 蔡国荣姜宝仅陈旻
Owner SHANGHAI CHEMSPEC CORP
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