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Synthesis process for ethoxy carbonyl isothiocyanate

A technology of ethoxycarbonyl isothiocyanate and synthesis process, which is applied in the field of ethoxycarbonyl isothiocyanate synthesis process, can solve the problems of serious environmental pollution and high production cost, and reduce environmental pollution and consumption , the effect of reducing energy loss

Active Publication Date: 2015-07-08
SHENYANG YOUYAN MINERAL CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Aiming at the problems of serious environmental pollution and high production cost, the invention provides a synthesis process of ethoxycarbonyl isothiocyanate

Method used

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  • Synthesis process for ethoxy carbonyl isothiocyanate

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Embodiment 1

[0010] In the ethoxycarbonyl isothiocyanate synthesis process of the present invention, 45 parts of sodium thiocyanate with a purity of 99% are dissolved in 80 parts of water, and 0.55 parts of polyethylene glycol with an average molecular weight of 200 are added to the solution. Diol, the temperature of the solution is lowered to below 10°C, and 54.8 parts of ethyl chloroformate with a purity of 99% are slowly added to the reaction system under stirring. The reaction temperature does not exceed 15°C, and the reaction is stirred for 3 hours. After the reaction, add 30 parts of water, stir for 10 minutes, and stand for 1 hour to separate the lower water phase. The upper oily liquid is N-ethoxycarbonyl isothiocyanate Ester, the product yield based on ethyl chloroformate is 83.42%, utilize this catalytic synthetic route to synthesize a series of products of alkoxycarbonyl isothiocyanate and carry out the next step of synthesizing alkoxy with the product synthesized by this synthet...

Embodiment 2

[0012] In the synthesis process of ethoxycarbonyl isothiocyanate of the present invention, 45 parts of sodium thiocyanate with a purity of 99% are dissolved in 80 parts of water, and 0.55 parts of polyethylene with an average molecular weight of 400 are added to the solution. Diol, the temperature of the solution is lowered to below 10°C, and 54.8 parts of ethyl chloroformate with a purity of 99% are slowly added to the reaction system under stirring. The reaction temperature does not exceed 15°C, and the reaction is stirred for 3 hours. After the reaction, add 30 parts of water, stir for 10 minutes, and stand for 1 hour to separate the lower water phase. The upper oily liquid is N-ethoxycarbonyl isothiocyanate Ester, the product yield based on ethyl chloroformate is 83.42%, utilize this catalytic synthetic route to synthesize a series of products of alkoxycarbonyl isothiocyanate and carry out the next step of synthesizing alkoxy with the product synthesized by this synthetic r...

Embodiment 3

[0014] In the ethoxycarbonyl isothiocyanate synthesis process of the present invention, 45 parts of sodium thiocyanate with a purity of 99% are dissolved in 80 parts of water, and 0.55 parts of polyethylene glycol with an average molecular weight of 600 are added to the solution. Diol, the temperature of the solution is lowered to below 10°C, and 54.8 parts of ethyl chloroformate with a purity of 99% are slowly added to the reaction system under stirring. The reaction temperature does not exceed 15°C, and the reaction is stirred for 3 hours. After the reaction, add 30 parts of water, stir for 10 minutes, and stand for 1 hour to separate the lower water phase. The upper oily liquid is N-ethoxycarbonyl isothiocyanate Ester, the product yield based on ethyl chloroformate is 83.42%, utilize this catalytic synthetic route to synthesize a series of products of alkoxycarbonyl isothiocyanate and carry out the next step of synthetic alkoxy with the product synthesized by this synthetic ...

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Abstract

Belonging to the technical field of chemical product synthesis and beneficiation reagent production, the invention in particular relates to a synthesis process for ethoxy carbonyl isothiocyanate. The process includes: dissolving 45 parts of 99% sodium thiocyanate in 80 parts of water, adding 0.55 part of polyethylene glycol with an average molecular weight of 200 into the solution, lowering the temperature of the solution to less than 10DEG C, adding 54.8 parts of 99% ethyl chloroformate slowly into the reaction system under stirring, controlling the reaction temperature not higher than 15DEG C, and carrying out stirring reaction for 3h, at the end of the reaction, adding 30 parts of water, performing stirring for 10min, then conducting standing for 1h, separating a lower layer water phase so as to obtain an upper layer oily liquid, i.e. N-ethoxy carbonyl isothiocyanate. The ethyl chloroformate based product yield is 83.42%, the environmental pollution is reduced, energy consumption is also lowered, and the catalyst dosage is reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical product synthesis and beneficiation agent production, and specifically relates to a synthesis process of ethoxycarbonyl isothiocyanate. Background technique [0002] Alkoxycarbonyl isothiocyanate, alkoxycarbonyl isothiocyanate synthesized by American Bayer Company and Cyanamide Company respectively adopts N,N-dialkylarylamine, quinoline, pyridine, etc. containing one or two nitrogen atoms The six-unit ring or ten-membered condensed polycyclic aromatic heterocyclic compounds are used as catalysts. Most of these catalysts are poisonous. At present, Schiff bases and their complexes have been widely used in the field of catalysts. Schiff's base is an efficient and low-toxic catalyst for alkoxycarbonyl isothiocyanate, but because the catalyst preparation process is complicated, and the reaction needs to be carried out under the situation that strong nucleophiles such as cyclohexanone are used as solve...

Claims

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Application Information

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IPC IPC(8): C07C331/32
Inventor 王咏梅张海龙牟松郭靖宇汪世跃
Owner SHENYANG YOUYAN MINERAL CHEM CO LTD
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