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Preparation method of tert-butyl arsenic

A technology of tert-butyl arsenic dichloride and tert-butyl, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, magnesium organic compounds, etc., can solve the problem of high cost and transportation of tert-butyl arsine Difficulty, poor safety and other problems, to achieve the effect of reducing the burden of purification, improving reaction efficiency, and reducing the burden of purification

Pending Publication Date: 2021-01-01
广东先导微电子科技有限公司
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Problems solved by technology

The disadvantage of this method is: the residual amount of magnesium in the process of synthesizing tert-butylmagnesium chloride by Grignard reaction method is too much, the yield is low, and there are many impurities; Arsenic chloride cannot fully participate in the reaction, resulting in the generation of highly toxic arsine in the next reduction; the crude tert-butyl arsenic has more impurities, and tert-butyl magnesium chloride has poor stability and difficult transportation, so tert-butyl magnesium chloride is directly used to prepare tert-butyl magnesium chloride Base arsine has high cost and poor safety

Method used

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  • Preparation method of tert-butyl arsenic

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preparation example Construction

[0030] The present invention provides a kind of preparation method of tert-butyl arsenic, described method comprises the following steps:

[0031] (1) Under the protection of an inert gas, magnesium and tert-butyl chloride react at 60°C to 80°C to generate tert-butylmagnesium chloride, and the reaction between magnesium and tert-butyl chloride is carried out under the condition of an initiator, and the initiator is Organic aluminum or inorganic aluminum, the weight ratio of the initiator to magnesium is (3-7):100, and the mass ratio of magnesium to tert-butyl chloride is 1.02:1-1.05:1;

[0032] (2) After arsenic trichloride and the tert-butylmagnesium chloride obtained in step (1) are stirred and reacted below 10°C, tert-butyl arsenic dichloride is obtained; the arsenic trichloride and the tert-butyl magnesium chloride obtained in step (1) The molar ratio of the base magnesium chloride is 0.5:1~0.9:1;

[0033] (3) The tert-butyl arsenic dichloride obtained in step (2) and the...

Embodiment 1

[0036] A kind of preparation method of tert-butyl arsenic as the embodiment of the present invention, described method comprises the following steps:

[0037] (1) Mix 35.1g magnesium bars, 450mL diethylene glycol dibutyl ether, and 1.76g aluminum chloride tetrahydrofuran complex to obtain reaction system B, remove the oxygen in reaction system B, and under nitrogen protection, react system B Heat to 75°C, add tert-chlorobutane solution dropwise to the stirred reaction system B with a constant pressure funnel, the chloro-tert-butane solution consists of 148mL chloro-tert-butane and 150mL diethylene glycol dibutyl Ether composition, insulated and stirred for 1.5 hours to obtain tert-butylmagnesium chloride, cooled to room temperature;

[0038] (2) Dissolve 180g of arsenic trichloride in 150mL of diethylene glycol dibutyl ether to obtain a reaction system C, cool the reaction system C to -10°C, keep the reaction system C in a stirring state, and drop it into the reaction system C...

Embodiment 2

[0042] As a preparation method of tert-butylarsenic in the embodiment of the present invention, the only difference between this embodiment and Embodiment 1 is that the initiator is anhydrous aluminum trichloride.

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Abstract

The invention provides a preparation method of tert-butyl arsenic, which comprises the following steps that (1) under the protection of inert gas, magnesium and chlorotert-butane react at 60-80 DEG Cto generate tert-butyl magnesium chloride, carrying out the reaction of magnesium and chlorotert-butane under the condition of an initiator, wherein the initiator is organic aluminum or inorganic aluminum, and the weight ratio of the initiator to magnesium is (3-7): 100; (2) stirring and reacting arsenic trichloride and tert-butyl magnesium chloride at the temperature of 10 DEG C or below to obtain tert-butyl arsenic dichloride; (3) stirring tert-butyl arsenic dichloride and a reducing agent to react at the temperature of 10 DEG C or below to obtain a tert-butyl arsenic crude product; (4) purifying the tert-butyl arsenic crude product obtained in the step (3). According to the method, the reaction efficiency of magnesium and chlorotert-butane is improved, the purity of the intermediate product tert-butyl magnesium chloride is improved, the conversion rate of arsenic trichloride is increased, and arsenic trichloride is prevented from generating side reaction to generate arsine in subsequent reaction, and therefore the purity of the crude tert-butyl arsenic product is improved.

Description

technical field [0001] The invention relates to the field of organometallic synthesis, in particular to a preparation method of tert-butyl arsenic. Background technique [0002] US2005 / 0033073 discloses a method for preparing tert-butylarsine, comprising the following process, synthesizing tert-butylmagnesium chloride by Grignard reaction; tert-butylmagnesium chloride reacts with arsenic chloride to synthesize tert-butyl arsenic dichloride; tert-butyl The crude product tert-butylarsine was synthesized by the reduction reaction of arsenic dichloride; the pure product tert-butyl arsine was obtained by adding a purifying agent for rectification and purification. The disadvantage of this method is: the residual amount of magnesium in the process of synthesizing tert-butylmagnesium chloride by Grignard reaction method is too much, the yield is low, and there are many impurities; Arsenic chloride cannot fully participate in the reaction, resulting in the generation of highly toxi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/72C07F3/02
CPCC07F9/72C07F3/02
Inventor 郭高伟陈世栋徐成曾翼俊欧立杰
Owner 广东先导微电子科技有限公司
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