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A kind of preparation method of trimethylsilyl trifluoromethanesulfonate

A technology of trimethylsilyl trifluoromethanesulfonate and trimethylsilanol, which is applied in the direction of silicon organic compounds, and can solve the problem of low quality of trimethylsilyl trifluoromethanesulfonate products

Active Publication Date: 2016-08-17
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] For the defect that the product quality of trimethylsilyl trifluoromethanesulfonate prepared by the current method is not high, the purpose of the present invention is to provide a kind of preparation method of trimethylsilyl trifluoromethanesulfonate

Method used

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  • A kind of preparation method of trimethylsilyl trifluoromethanesulfonate
  • A kind of preparation method of trimethylsilyl trifluoromethanesulfonate
  • A kind of preparation method of trimethylsilyl trifluoromethanesulfonate

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Comparison scheme
Effect test

Embodiment 1～15

[0062] Product detection method in following embodiment 1~15:

[0063] The obtained product was analyzed qualitatively and quantitatively by a Bruker 300 MHz nuclear magnetic resonance spectrometer. The product described below refers to a product whose composition is mainly trimethylsilyl trifluoromethanesulfonate after distillation of the reaction mixture.

[0064] The fluorine spectrum is the in situ spectrum of the pure product, and the hydrogen spectrum uses CDCl 3 as a solvent.

Embodiment 1

[0066] Step 1: In a 1000mL three-neck round bottom flask, add 350g of trifluoromethanesulfonyl chloride, and drop 185mL of trimethylsilanol into trifluoromethanesulfonyl chloride with a constant pressure dropping funnel, and the time for adding trimethylsilanol is 0.5 Hours, the molar ratio of trifluoromethanesulfonyl chloride and trimethylsilanol is 1.00:0.80, the reaction temperature is -50 ° C, stirring, HCl gas escapes, and the generated HCl gas is absorbed with NaOH solution. Stirring was continued, and the reaction time was 10 hours. After the reaction was completed, a reaction mixture was obtained.

[0067] Step 2: The reaction mixture was distilled under reduced pressure. After the distillation pressure was reduced to 0.030 MPa, the temperature of the reaction mixture was raised to 40° C. and stirred for 0.5 hour to remove unreacted trifluoromethanesulfonyl chloride. Then the temperature of the reaction mixture was raised to 70° C., stirred for 0.5 hour, and trimethyls...

Embodiment 2

[0070] Step 1: In a 1000mL three-neck round bottom flask, add 350g of trifluoromethanesulfonyl chloride, drop 243mL of trimethylsilanol into the trifluoromethanesulfonyl chloride with a constant pressure dropping funnel, and add trimethylsilanol for 0.5 Hours, the molar ratio of trifluoromethanesulfonyl chloride and trimethylsilanol is 1.00:1.05, the reaction temperature is 10 ° C, stirring, HCl gas escapes, and the generated HCl gas is absorbed with NaOH solution. Stirring was continued, and the reaction time was 4 hours. After the reaction was completed, a reaction mixture was obtained.

[0071] Step 2: The reaction mixture was distilled under reduced pressure. After the distillation pressure was reduced to 0.015 MPa, the temperature of the reaction mixture was raised to 40° C. and stirred for 0.5 hour to remove unreacted trifluoromethanesulfonyl chloride. The temperature of the reaction mixture was raised to 70° C., stirred for 0.5 hours, and trimethylsilanol was removed. F...

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Abstract

The invention relates to a preparation method of Trimethylsilyl trifluoromethanesulfonate, and belongs to the field of a fine chemical industry. The preparation method comprises the following specific steps: a compound of which the general formula is CF3SO2X reacts with hydroxytrimethylsilane, wherein X is Cl, F or OSO2CF3, and hydroxytrimethylsilane is used as a silicon alkylation reagent of the reaction; the reduced pressure distillation is carried out on a reaction mixture after the reaction is finished to collect Trimethylsilyl trifluoromethanesulfonate of which the mass content is higher than 99.0%, wherein the mole ratio of the CF3SO2X to the hydroxytrimethylsilane in the reaction is (1.00: 0.80) to (1.00: 1.60), the reaction time is 1 to 10 hours, the reduced pressure distillation is carried out on the reaction mixture after the reaction is finished, and the pressure is 0.005 to 0.030MPa.

Description

technical field [0001] The invention relates to a preparation method of trimethylsilyl trifluoromethanesulfonate, which belongs to the field of fine chemicals. Background technique [0002] Silyl trifluoromethanesulfonate derivatives are an important class of pharmaceutical intermediates, mainly including trimethylsilyl trifluoromethanesulfonate, tert-butyldimethylsilyl trifluoromethanesulfonate, trifluoromethanesulfonic acid Triisopropyl silicon ester, triethyl silicon trifluoromethanesulfonate, etc. Among them, trimethylsilyl trifluoromethanesulfonate is the most widely used. [0003] Trimethylsilyl Trifluoromethanesulfonate CF 3 SO 3 Si(CH 3 ) 3 , the English name is Trimethylsilyltrifluoromethanesulfonate, and its physical properties are shown in Table 1. [0004] The physical properties of table 1 trimethylsilyl trifluoromethanesulfonate [0005] [0006] Trimethylsilyl trifluoromethanesulfonate is a very effective methyl silylation reagent, which can be used ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/08
Inventor 黄华璠彭立培杨献奎徐海云李翔宇岳立平吕灵华
Owner PERIC SPECIAL GASES CO LTD
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