Methods for preparing N-alkoxycarbonyl isothiocyanate and derivative thereof
A technology of alkoxycarbonyl isothiocyanate and its derivatives, which is applied in the field of preparation of isothiocyanate and its derivatives, can solve the problems of low reaction efficiency, difficulty in catalyst removal, high catalyst toxicity, etc., and achieve catalytic High efficiency, non-toxic catalyst, and less waste water generation
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[0035] Example 1 Preparation of N-ethoxycarbonyl isothiocyanate
[0036] Dissolve 2.5 parts of N-(N',N'-dimethylaminopropyl)methyl isobutylimine with a purity of 99% in 200 parts of cyclohexane, and add 45.3 parts of thiocyanate with a purity of 98.5% Sodium, cool the mixture to a temperature of 0°C to 5°C with stirring. Under this temperature range and stirring, 54.3 parts of ethyl chloroformate with a purity of 98.5% were added to the reaction mixture, stirred and reacted for 3 hours, and the reaction was completed. Add 100 parts of water to dissolve the sodium chloride precipitate generated by the reaction, and separate the water phase to remove the water phase. The oil phase is distilled under reduced pressure to remove the solvent cyclohexane to obtain the desired N-ethoxycarbonyl isothiocyanate product. Analysis showed that the yield of the product based on ethyl chloroformate was 98.4%.
Example Embodiment
[0037] Example 2 Preparation of N-ethoxycarbonyl-0-ethylthiocarbonyl carbamate
[0038] The N-ethoxycarbonyl isothiocyanate product prepared according to Example 1 was added to 115 parts of ethanol while maintaining the temperature of the reaction mixture between about 25°C and about 45°C. The reaction mixture was then stirred at a temperature of about 40°C to 45°C for about 2 hours. The resulting product is an ethanol solution of N-ethoxycarbonyl-0-ethylthiocarbonyl carbamate. Analysis showed that the yield of the product based on ethyl chloroformate was 95.6%.
Example Embodiment
[0039] Example 3 Preparation of N-ethoxycarbonyl-0-isopropylthiocarbonyl carbamate (one-pot method)
[0040] Add 28 parts of N-(N',N'-dimethylaminopropyl) cyclohexanimine with a purity of 98% to 453 parts of NaSCN with a purity of 98% in 1000 parts of acetone, and then keep the temperature under stirring Between 10°C and about 25°C. 550 parts of 98.5% ethyl chloroformate were added to the reaction mixture in this temperature range and stirring. After the addition step, the reaction mixture is stirred and reacted at about 10°C to about 25°C for 4 hours to obtain N-ethoxycarbonyl isothiocyanate. Then, maintaining the reaction temperature between 10°C and 25°C, 491 parts of isopropanol was added with stirring. After the addition is complete, continue to stir and react for about 3 hours at a temperature of 45°C to 55°C, and the reaction is complete. The obtained mixture was washed with water, the aqueous phase was separated by liquid separation, and then the remaining acetone solv...
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