Method for synthesizing ethyl N-methyl cyanocarbamate by methylation reagent

A technology of ethyl cyanocarbamate and ethyl cyanocarbamate, which is applied in the field of methylating reagents to synthesize ethyl N-methylcyanocarbamate, and can solve problems such as potential safety hazards and corrosion of wastewater treatment facilities and equipment

Inactive Publication Date: 2020-10-27
XINYI AGRI CHEM PLANT JIANGSU PROV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In this synthesis method, the dimethyl sulfate that does not participate in the reaction will be dissolved in the waste water, and hydrolyze acid backlash ...

Method used

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  • Method for synthesizing ethyl N-methyl cyanocarbamate by methylation reagent
  • Method for synthesizing ethyl N-methyl cyanocarbamate by methylation reagent
  • Method for synthesizing ethyl N-methyl cyanocarbamate by methylation reagent

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Add 140g (1mol) of 30% cyanamide solution and 114g (1.05mol) of ethyl chloroformate into a 1000mL reaction flask equipped with a mechanical stirring device and a thermometer, start stirring, control the temperature in the reaction flask at 10-30°C, drop Add 30% sodium hydroxide solution until the pH value is 6.0, raise the temperature to 30-50°C and keep it warm for 3h. Then the temperature was lowered to 20-30° C., 99 g (1.1 mol) of dimethyl carbonate was added dropwise, and after the dropwise addition, the temperature was raised to 30-50° C. and kept for 3 hours. After the heat preservation was completed, it was cooled to room temperature, and transferred to a separatory funnel for static layering. The waste water in the lower layer was separated to obtain ethyl N-methylcyanocarbamate with a content of 97% and a yield of 95%.

Embodiment 2

[0033] Add 140g (1mol) of 30% cyanamide solution and 108.5g (1mol) of ethyl chloroformate into a 1000mL reaction flask equipped with a mechanical stirring device and a thermometer, start stirring, control the temperature in the reaction flask at 10-30°C, drop Add 30% sodium hydroxide solution until the pH value is 7.0, raise the temperature to 30-50°C and keep it warm for 3h. Then the temperature was lowered to 20-30° C., 90 g (1 mol) of dimethyl carbonate was added dropwise, and after the dropwise addition, the temperature was raised to 30-50° C. and kept for 3 hours. After the heat preservation was completed, it was cooled to room temperature, and transferred to a separatory funnel for static layering. The waste water in the lower layer was separated to obtain ethyl N-methylcyanocarbamate with a content of 95% and a yield of 93%.

Embodiment 3

[0035] Add 140g (1mol) of 30% cyanamide solution and 110.7g (1.02mol) of ethyl chloroformate into a 1000mL reaction flask equipped with a mechanical stirring device and a thermometer, start stirring, and control the temperature in the reaction flask at 10-30°C. 50% sodium hydroxide solution was added dropwise until the pH value was 7.0, and the temperature was raised to 30-50° C. for 3 hours. Then the temperature was lowered to 20-30° C., 94.5 g (1.05 mol) of dimethyl carbonate was added dropwise, and after the dropwise addition, the temperature was raised to 30-50° C. and kept for 3 hours. After the heat preservation was completed, it was cooled to room temperature, and transferred to a separatory funnel for static layering. The waste water in the lower layer was separated to obtain ethyl N-methylcyanocarbamate with a content of 96% and a yield of 94%.

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Abstract

The invention discloses a method for synthesizing ethyl N-methyl cyanocarbamate by using a methylation reagent. The method comprises the following steps of: 1) reacting cyanamide with ethyl chloroformate under a strong alkali condition to generate ethyl cyanocarbamate; and 2) carrying out reaction on ethyl cyanocarbamate and a methylation reagent dimethyl carbonate under a strong alkaline condition to generate ethyl N-methyl cyanocarbamate. According to the new method for synthesizing the ethyl N-methyl cyanocarbamate by using the methylation reagent, the low-toxicity and safe methylation reagent dimethyl carbonate is used for replacing dimethyl sulfate; the method is safer, can overcome the problem of equipment corrosion caused by acid regurgitation of wastewater in the conventional method, and has the advantages of more stable reaction, few byproducts, higher yield and stronger operability.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for synthesizing ethyl N-methylcyanocarbamate with a methylating reagent. Background technique [0002] N-methyl cyanocarbamate can usually be used as an intermediate to synthesize hexazinone. For example, patents CN20S0603A03755654A and US4178448 describe the synthetic method of N-methyl cyanocarbamate in detail. Above-mentioned patents all use dimethyl sulfate as Methylation reagent, i.e. ethyl cyanocarbamate and dimethyl sulfate are alkylated to synthesize N-methyl ethyl cyanocarbamate under the effect of strong base, and the reaction formula is as follows: [0003] [0004] In this synthesis method, the dimethyl sulfate that does not participate in the reaction will be dissolved in the waste water, and hydrolysis and acid backlash will occur rapidly under the condition of 50°C, corroding the waste water treatment facilities and equipment; meanwhile, the dimethyl s...

Claims

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Application Information

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IPC IPC(8): C07C261/04
CPCC07C261/04
Inventor 顾思雨邓玉智杨海松佟林朱新江
Owner XINYI AGRI CHEM PLANT JIANGSU PROV
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