Synthesis process and synthesis equipment for mixture of buprofezin intermediate tert-butyl thiocyanate and tert-butyl isocyanate

A technology of bulk thiocyanate and synthesis process, which can be used in the preparation of isocyanic acid derivatives, the preparation of organic compounds, chemical instruments and methods, etc. Carbon disulfide, the effect of improving stability and improving product quality

Pending Publication Date: 2021-04-23
JIANGSU ANPON ELECTROCHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to provide a synthesis process and synthesis equipment of a mixture of buprofezin intermediate tert-butyl thiocyanate and tert-butyl isocyanate, aiming to solve the problem of sulfur Ammonium cyanate decomposes more, so it leads to the technical problem of excessive carbon disulfide content in the product

Method used

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  • Synthesis process and synthesis equipment for mixture of buprofezin intermediate tert-butyl thiocyanate and tert-butyl isocyanate
  • Synthesis process and synthesis equipment for mixture of buprofezin intermediate tert-butyl thiocyanate and tert-butyl isocyanate
  • Synthesis process and synthesis equipment for mixture of buprofezin intermediate tert-butyl thiocyanate and tert-butyl isocyanate

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Example 1, see figure 1 , the present invention provides a technical solution: a synthesis process of a mixture of buprofezin intermediate tert-butyl thiocyanate and tert-butyl isocyanate, comprising the following steps:

[0027] S1: Ammonium thiocyanate 76g (1.0mol) is joined in the water of 80g, stir until it dissolves;

[0028] S2: After completely dissolving, add 76.2g (1.03mol) of tert-butanol, then add 0.3g (0.002mol) of 2-tert-butylaniline to obtain a mixed solution, and slowly raise the temperature of the mixed solution to 60°C;

[0029] S3: Slowly add 105 g (1.05 mol) of concentrated hydrochloric acid dropwise to the heated mixed solution, and after the dropwise addition is completed, the temperature is raised to 80° C. and kept for 6 hours;

[0030] S4: After the heat preservation is completed, the stirring is turned off and the stratification is static, and the mixture of tert-butyl thiocyanate and tert-butyl isocyanate is obtained by washing twice.

[0031...

Embodiment 2

[0035] Example 2, see figure 2 , the present invention provides a technical solution: a synthesis process of a mixture of buprofezin intermediate tert-butyl thiocyanate and tert-butyl isocyanate, comprising the following steps:

[0036] S1: Ammonium thiocyanate 76g (1.0mol) is joined in the water of 80g, stir until it dissolves;

[0037] S2: After complete dissolution, add 76.2g (1.03mol) of tert-butanol, then add 0.12g (0.002mol) of acetamide to obtain a mixed solution, and slowly raise the temperature of the mixed solution to 60°C;

[0038] S3: Slowly add 105 g (1.05 mol) of concentrated hydrochloric acid dropwise to the heated mixed solution, and after the dropwise addition is completed, the temperature is raised to 80° C. and kept for 6 hours;

[0039] S4: After the heat preservation is completed, the stirring is turned off and the stratification is static, and the mixture of tert-butyl thiocyanate and tert-butyl isocyanate is obtained by washing twice.

[0040] Wherein...

Embodiment 3

[0044] Example 3, see image 3 , the present invention provides a technical solution: a synthesis process of a mixture of buprofezin intermediate tert-butyl thiocyanate and tert-butyl isocyanate, comprising the following steps:

[0045] S1: Ammonium thiocyanate 76g (1.0mol) is joined in the water of 80g, stir until it dissolves;

[0046] S2: After completely dissolving, add 77.7g (1.05mol) of tert-butanol, then add 0.3g (0.002mol) of 2-tert-butylaniline to obtain a mixed solution, and slowly raise the temperature of the mixed solution to 60°C;

[0047] S3: Slowly add 110 g (1.1 mol) of concentrated hydrochloric acid dropwise to the heated mixed solution, and after the dropwise addition is completed, the temperature is raised to 80° C. and kept for 6 hours;

[0048] S4: After the heat preservation is completed, the stirring is turned off and the stratification is static, and the mixture of tert-butyl thiocyanate and tert-butyl isocyanate is obtained by washing twice.

[0049]...

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Abstract

The invention discloses a synthesis process and synthesis equipment for a mixture of buprofezin intermediate tert-butyl thiocyanate and tert-butyl isocyanate. The process comprises the following steps of: adding ammonium thiocyanate into water, adding tert-butyl alcohol at normal temperature, performing heating to 60-75DEG C, adding an ammonium thiocyanate stabilizer, slowly adding concentrated hydrochloric acid dropwise, controlling the dropwise adding time at 2-6h, performing heating to 75-90DEG C, and keeping the temperature for 2-4h, and controlling the molar mass ratio of ammonium thiocyanate to tert-butyl alcohol to concentrated hydrochloric acid at 1:1-1.1:1-1.2; and carrying out water separation on the reaction product, and carrying out secondary water washing to obtain a mixture (mixed ester for short) of tert-butyl thiocyanate and tert-butyl isocyanate. The method has the beneficial effects that: the process is simple, the product quality is relatively high, and the content of carbon disulfide in the mixed ester is greatly reduced.

Description

technical field [0001] The invention relates to the technical field of pesticide synthesis, in particular to a synthesis process and synthesis equipment for a mixture of buprofezin intermediate tert-butyl thiocyanate and tert-butyl isocyanate. Background technique [0002] Pililing is a new type of insect growth regulator with high efficiency, long duration, strong selectivity and safety. It is mainly used for the control of leafhoppers, planthoppers, whiteflies and scale insects in crops such as rice, vegetables, tea and citrus. It is currently the leading species for the control of rice planthoppers; Ammonium phosphate is used as raw material to react with tert-butanol in the presence of hydrochloric acid to obtain a mixture of tert-butyl thiocyanate and tert-butyl isocyanate (referred to as mixed ester), and through transposition to obtain tert-butyl isothiocyanate (referred to as isoester) , and then react with isopropylamine to obtain thiourea. Finally, the chloride an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C263/00C07C265/04C07C331/04
Inventor 姚修宇范锦龙杨玉坤徐晓东李卫陈建国姜育田朱学军唐素荣万金方于同锋
Owner JIANGSU ANPON ELECTROCHEM
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