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Preparation method of triisopropyl silicon-based trifluoromethanesulfonate

A technology of propylsilyl trifluoromethanesulfonate and trifluoromethanesulfonic acid is applied in the field of preparation of triisopropylsilyl trifluoromethanesulfonate, and can solve the problems of difficult separation of rectification methods, and the like, To achieve the effect of easy operation

Pending Publication Date: 2022-04-26
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing triisopropylsilyl trifluoromethanesulfonate synthesis method is mainly prepared by the reaction of trifluoromethanesulfonic acid and triisopropylsilane, and there will be rearrangement by-products in addition to the main product in the reaction process, The boiling point is close to triisopropylsilyl trifluoromethanesulfonate, it is difficult to separate by rectification

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The preparation method of the triisopropylsilyl trifluoromethanesulfonate of the present embodiment, the method is:

[0017] S1. Put 70.8g (0.47mol, 1.0eq.) of trifluoromethanesulfonic acid into a three-necked flask with a thermometer, a constant pressure dropping funnel and a condenser tube, replace the reaction system three times with nitrogen, and put 100g ( 0.52mol, 1.1eq.) Triisopropyl halosilane is dropped into a three-necked flask through a constant pressure dropping funnel at a rate of 1 drop / second, added to trifluoromethanesulfonic acid, and stirred at a temperature of 60°C While heating, continue to stir for 15 hours after the dropwise addition to obtain a mixture of triisopropylsilyl trifluoromethanesulfonate and triisopropyl halosilane; the halogen in the triisopropyl halosilane is Cl;

[0018] S2. Distill the mixture of triisopropylsilyl trifluoromethanesulfonate and triisopropyl halosilane obtained in S1 under reduced pressure at a pressure of -0.099MPa, ...

Embodiment 2

[0020] The preparation method of the triisopropylsilyl trifluoromethanesulfonate of the present embodiment, the method is:

[0021] S1. Put 70.8g (0.47mol, 1.0eq.) of trifluoromethanesulfonic acid into a three-neck flask with a thermometer, a constant pressure dropping funnel, and a condenser, and replace the reaction system with nitrogen three times. (1.41mol, 3eq.) Triisopropyl halosilane is dropped into the three-necked flask through the constant pressure dropping funnel at a rate of 1 drop / 5 seconds, added to trifluoromethanesulfonic acid, and kept under the condition of 40°C Heating while stirring, and continuing to stir for 24 hours after the dropwise addition, to obtain a mixture of triisopropylsilyl trifluoromethanesulfonate and triisopropyl halosilane; the halogen in the triisopropyl halosilane is Cl;

[0022] S2. Distill the mixture of triisopropylsilyl trifluoromethanesulfonate and triisopropyl halosilane obtained in S1 under reduced pressure at a pressure of -0.095...

Embodiment 3

[0024] The preparation method of the triisopropylsilyl trifluoromethanesulfonate of the present embodiment, the method is:

[0025] S1. Put 141.2g (0.94mol, 1.0eq.) of trifluoromethanesulfonic acid into a three-necked flask with a thermometer, a constant pressure dropping funnel, and a condenser, and replace the reaction system with nitrogen three times. (1.88mol, 2.0eq.) Triisopropyl halosilane is dropped into the three-necked flask through the constant pressure dropping funnel at a rate of 1 drop / second, added to trifluoromethanesulfonic acid, and the temperature is 80°C. Heating while stirring, and continuing to stir for 8 hours after the dropwise addition was completed, to obtain a mixture of triisopropylsilyl trifluoromethanesulfonate and triisopropyl halosilane; the halogen in the triisopropyl halosilane is I;

[0026] S2. Distill the mixture of triisopropylsilyl trifluoromethanesulfonate and triisopropyl halosilane obtained in S1 under reduced pressure at a pressure of ...

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Abstract

The invention provides a preparation method of triisopropyl silicon-based trifluoromethanesulfonate, which comprises the following steps: dropwise adding triisopropyl halogenosilane into trifluoromethanesulfonic acid, heating while stirring at 40-80 DEG C, continuously stirring after dropwise adding to obtain a mixture of triisopropyl silicon-based trifluoromethanesulfonate and triisopropyl halogenosilane, carrying out reduced pressure distillation at-0.099--0.095 MPa, and carrying out reduced pressure distillation at-0.099--0.095 MPa to obtain triisopropyl silicon-based trifluoromethanesulfonate; and collecting the triisopropyl halogenosilane at 170 DEG C, and then collecting at 210-230 DEG C to obtain the triisopropyl silicon-based trifluoromethanesulfonate. According to the method, only the trifluoromethanesulfonic acid and the triisopropyl halogenosilane are used for reaction, no solvent is needed in the reaction, the redundant triisopropyl halogenosilane is rectified and recycled, and the method is simple, rapid and easy to operate.

Description

technical field [0001] The invention belongs to the technical field of preparation of triisopropylsilyl trifluoromethanesulfonate, and in particular relates to a preparation method of triisopropylsilyl trifluoromethanesulfonate. Background technique [0002] Triisopropylsilyl trifluoromethanesulfonate is a protective group of organic compounds and a reagent widely used in pesticides, pharmaceutical intermediates and organic materials. It is mainly used in the protection of aliphatic hydroxyl groups and aliphatic aldehydes and ketones. It is a good isopropyl silylation reagent; in organic synthesis, it participates in the growth of carbon-carbon bonds in various organic compounds, and can also be used as a catalyst for certain reactions Catalysts, such as those used to catalyze the rearrangement of aryl epoxides. [0003] The existing triisopropylsilyl trifluoromethanesulfonate synthesis method is mainly prepared by the reaction of trifluoromethanesulfonic acid and triisopro...

Claims

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Application Information

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IPC IPC(8): C07F7/08
CPCC07F7/0834
Inventor 王巍姚刚花莹曦倪珊珊户帅帅吴昊俣姜世楠付志杰
Owner PERIC SPECIAL GASES CO LTD
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