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Preparation method of deuterated ammonia and deuteration reaction participated by deuterated ammonia as deuterium source

A deuterium and reaction technology, applied in the field of deuterated ammonia preparation and deuterated reaction, can solve the problems of high price and high energy consumption, and achieve the effects of low operating cost and mild reaction conditions.

Pending Publication Date: 2021-10-22
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In short, the preparation method of deuterated ammonia has the disadvantages of expensive equipment and high energy consumption.

Method used

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  • Preparation method of deuterated ammonia and deuteration reaction participated by deuterated ammonia as deuterium source
  • Preparation method of deuterated ammonia and deuteration reaction participated by deuterated ammonia as deuterium source
  • Preparation method of deuterated ammonia and deuteration reaction participated by deuterated ammonia as deuterium source

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Effect test

Embodiment 1

[0032] Get benzonitrile (0.5mmol), platinum nanowire (0.025mmol) and mix in 2mL deuterated methanol, pass into 2mmol deuterium gas, 40 ℃ stirring reaction for 4 hours, produce 0.23mmol deuterated ammonia, deuterated ammonia production rate is 92%. pass image 3 In the Raman test, it can be confirmed that the obtained is deuterated ammonia.

Embodiment 2

[0034] Take p-ethylbenzonitrile (0.5mmol) and platinum nanorods (0.05mmol) and mix them in 2mL deuterated benzene, pass through 2mmol ml of deuterium gas, stir and react at 50°C for 6 hours to produce 0.21mmol deuterated ammonia, deuterated Ammonia yield was 84%.

Embodiment 3

[0036] Take p-chlorobenzonitrile (1mmol) and palladium nanowires (0.05mmol) and mix them in 2mL of deuterated benzene, feed 3mmol of deuterium gas, stir and react at 35°C for 10 hours to produce 0.43mmol of deuterated ammonia, and the yield of deuterated ammonia is was 86%.

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Abstract

The invention provides a preparation method of deuterated ammonia and a rapid deuteration reaction participated by the deuterated ammonia as a deuterium source, and belongs to the technical field of organic synthesis. The preparation method of the deuterated ammonia comprises the following step of: obtaining the deuterated ammonia from a nitrile group compound under the action of a catalyst in a deuterium source atmosphere. According to the preparation method of the deuterated ammonia, the target product can be obtained in one step through simple organic reaction under mild conditions, and the operation is simple; and the generated deuterated ammonia can be directly used as the deuterium source, and is rapidly subjected to hydrogen-deuterium exchange reaction with active hydrogen to synthesize a corresponding deuterated compound. The active hydrogen-containing compound comprises a hydroxyl compound, a thiol compound, an alkynyl compound, a phenolic compound, a silicon-hydrogen compound or an amino compound. The method has the advantages of mild reaction conditions, low operation cost and wide universality.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a method for preparing deuterated ammonia and a deuterated reaction in which it is used as a deuterium source. Background technique [0002] Deuterated ammonia (ND 3 ) was first prepared by British chemist Hugh Stott Taylor in 1933 by reacting magnesium nitride with deuterium water. Deuterated ammonia is composed of one nitrogen atom and three deuterium atoms, and is a colorless gas with a pungent odor at room temperature. The economic value of deuterated ammonia is very high, and it has the characteristics of a wide range of applications, and plays a very important role in many fields. Since the observation of deuterated ammonia in the Barnard 1 nebula confirmed the important role of deuterated ammonia in the exploration of star formation, astronomers' research on deuterated ammonia has never stopped. Deuterated ammonia is used as a polarized solid target material i...

Claims

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Application Information

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IPC IPC(8): C01C1/08C07B59/00
CPCC01C1/08C07B59/001C07B2200/05
Inventor 郎建平顾宏伟朱峰源牛政
Owner SUZHOU UNIV
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