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Method for preparing deuterated acetonitrile through photoelectric integrated catalysis

A technology for the preparation of deuterated acetonitrile and catalysis, which is applied in the direction of organic chemical methods, chemical instruments and methods, and the preparation of organic compounds. Low generation cost, short response time, and easy operation

Active Publication Date: 2022-07-22
安徽贵朋功能材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This traditional method often has disadvantages such as long time-consuming, high energy consumption, and low deuteration rate, which greatly increases the cost of deuterated acetonitrile
CN 114436893 A mentions the preparation of deuterated acetonitrile by using a nano-scale supported catalyst, but this method needs heating and takes a long time, and the preparation process of the catalyst is relatively cumbersome

Method used

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  • Method for preparing deuterated acetonitrile through photoelectric integrated catalysis
  • Method for preparing deuterated acetonitrile through photoelectric integrated catalysis
  • Method for preparing deuterated acetonitrile through photoelectric integrated catalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Add 10 mmol of acetonitrile to 100 mmol of deuterium water, and add a composite catalyst (deuterated DMSO: 5 mmol, H 2 SO 4 : 0.1 mmol, TiO 2 : 0.1 mmol, tetrabutylammonium tetrafluoroborate: 0.5 mmol, NaB 6 H 7 : 0.1 mmol), N 2 Stir well under protection;

[0029](2) The power is 20W, the wavelength is 365nm UV lamp irradiation, C(+) / Pt(-) is used as the electrode, and the current is 10mA, and the reaction is fully reacted at 25℃ for 0.5h;

[0030] (3) After the reaction, the catalyst was collected by filtration, and the filtrate was distilled under reduced pressure at 40°C to obtain a crude deuterated acetonitrile;

[0031] (4) Using anhydrous Na 2 SO 4 After drying for 24 h, pure deuterated acetonitrile can be obtained with a yield of 99.10%, and its deuteration rate detected by high-resolution mass spectrometry is 99.92%. The nuclear magnetic contrast spectra before and after deuteration of acetonitrile are shown in the accompanying drawings ( figure 1 ...

Embodiment 2

[0033] (1) Add 1 mmol of acetonitrile to 5 mmol of deuterium water, and add a composite catalyst (deuterated DMSO: 0.08 mmol, FeCl 3 : 0.02 mmol, TiO 2 : 0.05 mmol, tetramethylammonium chloride: 0.03 mmol, Cs 2 B 8 H 8 : 0.025 mmol, B 10 H 14 : 0.025 mmol), N 2 Stir well under protection;

[0034] (2) The power is 5W, and the wavelength is 390nm UV lamp irradiation, C(+) / Pt(-) is used as the electrode, and the current is 15mA, and the reaction is fully reacted at 20℃ for 1 h;

[0035] (3) After the reaction, the catalyst was collected by filtration, and the filtrate was distilled under reduced pressure at 40°C to obtain a crude deuterated acetonitrile;

[0036] (4) Using anhydrous MgSO 4 After drying for 24 h, pure deuterated acetonitrile can be obtained with a yield of 99.21%, and its deuteration rate detected by high-resolution mass spectrometry is 99.86%.

Embodiment 3

[0038] (1) Add 5 mmol of acetonitrile to 100 mmol of deuterium water, and add a composite catalyst (deuterated DMSO: 0.25 mmol, AgNO 3 : 0.025mmol, TiO 2 : 0.05mmol, tetrabutylammonium hexafluorophosphate: 0.025mmol, C 2 B 10 H 12 : 0.05 mmol), N 2 Stir well under protection;

[0039] (2) The power is 25W, and the wavelength is 265nm under the irradiation of ultraviolet lamp, C(+) / Pt(-) is used as the electrode, and the current is 20mA, and the reaction is fully reacted at 15℃ for 2 hours;

[0040] (3) After the reaction, the catalyst was collected by filtration, and the filtrate was distilled under reduced pressure at 40°C to obtain a crude deuterated acetonitrile;

[0041] (4) Using anhydrous CaCl 2 After drying for 24 h, pure deuterated acetonitrile can be obtained with a yield of 99.43%, and its deuteration rate detected by high-resolution mass spectrometry is 99.91%.

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Abstract

The invention discloses a method for efficiently preparing deuterated acetonitrile by photoelectric integrated catalysis, which is characterized in that deuterium water which is cheapest and easy to obtain is used as a deuterium source, acetonitrile is used as a raw material, and a plurality of catalysts are used for synergism to react at room temperature for a plurality of hours. And after the reaction is finished, carrying out reduced pressure distillation and drying to obtain the deuterated acetonitrile. The deuteration rate of the deuterated acetonitrile is greater than 99.8% through high-resolution mass spectrometry detection, and the deuterated acetonitrile meets the standard of commercial deuterated acetonitrile.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a method for preparing deuterated acetonitrile by novel photoelectric integrated catalysis. Background technique [0002] Deuterated acetonitrile is an organic solvent that can be used as an aprotic solvent for organic reactions. At the same time, deuterated acetonitrile is also one of the most commonly used nuclear magnetic (NMR) detection solvents. At present, its main preparation method is to remove -CH in acetonitrile under the action of strong alkali and high temperature. 3 protons, D in deuterium water + An electrophilic reaction occurs, thereby completing the H-D exchange. The traditional method is often time-consuming, high energy consumption, low deuteration rate and other shortcomings, which greatly increases the cost of deuterated acetonitrile. CN 114436893 A mentioned the use of nano-scale supported catalyst to prepare deuterated acetonitrile, but this method requ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C253/34C07C255/03C07B59/00C25B3/09C25B3/20C25B3/21B01J31/38
CPCC07C253/30C07C253/34C07B59/001C25B3/09C25B3/20C25B3/21B01J31/38C07B2200/05B01J2231/40B01J35/33B01J35/39C07C255/03
Inventor 张海波漆斌陆静
Owner 安徽贵朋功能材料科技有限公司
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