Preparation method of perdeuterated methanol

A technology of fully deuterated methanol and deuterium gas, which is applied in the preparation of organic compounds, organic chemical methods, chemical instruments and methods, etc., can solve the problems of low total yield, harsh reaction conditions, complex process, etc., and improve the conversion rate and the yield of the product, the effect of improving the convenience of operation and mild reaction conditions

Active Publication Date: 2018-07-06
上海枢炬化工有限公司
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  • Abstract
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Problems solved by technology

[0003] However, the preparation method of ordinary methanol is not suitable for the preparation of perdeuterated methanol. In the currently published technical data, there are problems such as harsh reaction conditions, ...

Method used

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Embodiment 1

[0023] This embodiment provides a preparation method for fully deuterated methanol, specifically: open the valve of deuterium gas and carbon monoxide, control the volume ratio to 1:1 and pre-mix first (deuterium gas and carbon monoxide are 2kg and 14kg respectively, 16kg in total) . Under the pressure of 5.5MPa, at the speed of 2L / s, through the catalyst bed of gold oxide: platinum oxide: rhodium oxide = 1:3:2 (mass ratio) at 210~380°C, after continuous circulation reaction for 24 hours, in Separating the kettle to obtain the perdeuterated methanol reaction solution, the obtained reaction solution was rectified to obtain perdeuterated methanol: 3.2kg, the yield was 35.5%, and the GC purity was 99.8%. Elemental analysis theoretical value: C 33.30%, D22.34%, O44.36%; measured value: C 33.32%, D22.33%, O44.35%.

Embodiment 2

[0025] This embodiment provides a preparation method for fully deuterated methanol, specifically: open the valve of deuterium gas and carbon monoxide, control the volume ratio to 1:3 and pre-mix first (deuterium gas and carbon monoxide are 2kg and 42kg respectively, 44kg in total) . Under the pressure of 5.5MPa, at the speed of 2L / s, through the catalyst bed layer with a mass ratio of 210~380°C of gold oxide: platinum oxide: rhodium oxide = 1:3:2, after continuous circulation reaction for 24 hours, after separation The reaction liquid of perdeuterated methanol was obtained in the kettle, and the obtained reaction solution was rectified to obtain perdeuterated methanol: 8.1kg, the yield was 90%, and the GC purity was 99.8%. Elemental analysis theoretical value: C 33.30%, D22.34%, O44.36%; measured value: C 33.32%, D22.33%, O44.35%.

Embodiment 3

[0027] This embodiment provides a preparation method for fully deuterated methanol, specifically: open the valve of deuterium gas and carbon monoxide, control the volume ratio to 1:4 and pre-mix first (deuterium gas and carbon monoxide are 2kg and 56kg respectively, 58kg in total) . Under the pressure of 5.5MPa, at the speed of 2L / s, through the catalyst bed layer with a mass ratio of 210~380°C of gold oxide: platinum oxide: rhodium oxide = 1:3:2, after continuous circulation reaction for 24 hours, after separation The reaction solution of perdeuterated methanol was obtained in the still, and the obtained reaction solution was rectified to obtain perdeuterated methanol: 8.4kg, the yield was 93.3%, and the GC purity was 99.8%. Elemental analysis theoretical value: C 33.30%, D22.34%, O44.36%; measured value: C 33.32%, D22.34%, O44.34%.

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Abstract

The invention discloses a preparation method of perdeuterated methanol. The preparation method comprises the following step: taking deuterium and carbon monoxide to react in the presence of a catalystunder conditions that the reaction pressure is 1 to 10Mpa and the reaction temperature is 150 to 550 DEG C, so as to generate the perdeuterated methanol, wherein the feeding volume ratio of the deuterium to the carbon monoxide is 1 to (1 to 10) and the catalyst is selected from one or a combination of more of gold oxide, platinum oxide and rhodium oxide. The preparation method of the perdeuterated methanol, disclosed by the invention, has the advantages of moderate reaction conditions, high reaction yield and simple technological operation.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of perdeuterated methanol. Background technique [0002] Deuterated methanol is an important chemical raw material and deuterated drug intermediate. The structure shown in the perdeuterated methanol: CD 3 OD. In chemical synthesis, it is a commonly used proton nuclear magnetic resonance spectrum detection reagent, and is widely used in experimental research work. In recent years, since deuterated drugs have become a hot spot in drug research, deuterium methanol has also been widely used in the study of deuterated drugs. At present, there are many deuterium drugs in clinical research, such as deuterium tetrabenazine, deuterium venlafaxine, deuterium tofacitinib, deuterium instead of cagrel, deuterium pirfenidone, deuterium paroxetine , deuterated atazanavir and other deuterated drugs. [0003] However, the preparation method of ordinary methan...

Claims

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Application Information

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IPC IPC(8): C07C31/04C07C29/158C07C29/157C07C29/154C07B59/00
CPCC07B59/001C07B2200/05C07C29/154C07C29/157C07C29/158C07C31/04Y02P20/52
Inventor 刘世领姜艳钱永中
Owner 上海枢炬化工有限公司
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