Preparation method of trifluoroethyl trifluoromethanesulfonate

A technology of trifluoroethyl trifluoromethanesulfonate and trifluoromethanesulfonyl fluoride, which is applied in the field of preparation of organic synthesis intermediates, and can solve problems such as the preparation method of trifluoroethyl trifluoromethanesulfonate that has not been retrieved

Inactive Publication Date: 2019-05-14
NANTONG ZHENGDA AGROCHEM
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Problems solved by technology

[0003] But the preparation method of relevant trifluoroethyl trifluoromethanesulfonate has not been retrieved at present

Method used

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Embodiment 3

[0014] The preparation method of trifluoroethyl trifluoromethanesulfonate of present embodiment, this preparation method comprises the steps:

[0015] Step 1: Synthesis: Add 21kg of triethylamine into a dry and clean 200L kettle, turn on cooling water under stirring, control the temperature at 10-20°C, then add 20.6kg of trifluoroethanol dropwise into the kettle, and control the temperature at 25°C, dropwise time is 1h, stir for 20min after dropping, then cool down with ice-salt water to the temperature <10°C, then slowly pour 33kg of trifluoromethanesulfonyl fluoride into it, the temperature is controlled at 6-10°C, The time is 4.5-6 hours. The first four hours are based on the speed of no tail gas emission, about 6-7kg per hour, and the speed is slower in the latter; after the completion of the pass, stir for 3-4 hours, the temperature is 10-15 ° C, and the synthesis is over. ;

[0016] Step 2: Hydrolysis: Cool the material synthesized in step 1 to 10°C, then drop 45kg of w...

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Abstract

The invention relates to a preparation method of trifluoroethyl trifluoromethanesulfonate. The preparation method comprises the following steps: (1) synthesis: synthesizing triethylamine, trifluoroethanol and trifluoromethanesulfonyl fluoride to obtain a synthesized material; (2) hydrolysis: hydrolyzing the synthesized material; and (3) rectifying: feeding an organic matter obtained by hydrolysisinto a 300 L rectifying kettle, heating the organic matter with steam, and collecting a fraction, the tower top temperature and the boiling point of which is 89 DEG C, as a target product trifluoroethyl trifluoromethanesulfonate. The preparation method has the advantages that according to the preparation method of the trifluoroethyl trifluoromethanesulfonate, the content of the prepared trifluoroethyl trifluoromethanesulfonate can reach over 98% by selecting proper raw materials and controlling reaction conditions effectively, and the trifluoroethyl trifluoromethanesulfonate can be used for organic synthesis.

Description

technical field [0001] The invention belongs to the technical field of preparation of organic synthesis intermediates, in particular to a preparation method of trifluoroethyl trifluoromethanesulfonate. Background technique [0002] Trifluoroethyl trifluoromethanesulfonate, another name is 2,2,2-trifluoroethyl trifluoromethanesulfonate, the English name is TRIFLUOROMETHANESULFONIC ACID, the CAS number is 6226-25-1, and the molecular formula is C3H2F6O3S. It is used in Organic synthesis intermediates. [0003] But do not retrieve the preparation method of relevant trifluoromethanesulfonate trifluoroethyl ester at present. Contents of the invention [0004] The technical problem to be solved by the present invention is to provide a method for preparing trifluoroethyl trifluoromethanesulfonate, and the prepared trifluoroethyl trifluoromethanesulfonate can be used in organic synthesis. [0005] In order to solve the above-mentioned technical problems, the technical solution o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/66C07C303/28C07C303/44
Inventor 钱灿明
Owner NANTONG ZHENGDA AGROCHEM
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