Preparation method of trifluoroisothiocyanate ethane
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A technology of isothiocyanate and trifluoroethylamine is applied in the field of preparation of trifluoroisothiocyanate, can solve the problems of unsuitability for industrial production, low actual yield, low yield and the like, and achieves low toxicity, The effect of improving reaction yield and high yield
Pending Publication Date: 2021-06-22
ZHEJIANG HISUN CHEM
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However, although this reaction route avoids the use of highly toxic raw materials, the actual yield is low, and there are many three wastes, so it is not suitable for industrial production
[0006] In summary, in order to solve the problems of high cost, low yield, and many wastes in the prior art, it is urgent to develop a low-cost, high-yield, environmentally friendly, and industrialized production of trifluoroisothiocyanate The preparation method of alkane meets the increasing demand for industrial production
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Embodiment 1
[0020] Embodiment 1: drop into 40.0g trifluoroethylamine (0.404mol, 1eq), 47.0g triethylamine (0.465mol, 1.15eq) and 130.0g toluene (1.411mol) in the round bottom bottle, stir and cool to 10-12 ℃, slowly add 33.5g of carbon disulfide (0.440mol, 1.09eq) dropwise, after the dropwise completion, react at a temperature of 10℃ for 10 hours to obtain trifluoroethylaminothioformate. Then lower the temperature to 5-10°C, slowly add 139.0g of solid light-toluene mixed solution (containing 0.154mol of solid light, 0.38eq; toluene 1.013mol) dropwise, and stir at room temperature for 2 hours, then heat up to 40-45°C (Act to remove fixed light) react for 3 hours. After the sampling test is qualified (trifluoroethylamine content ≤ 0.5%), the temperature of the reaction solution is lowered to 5-10°C, water is added, stirred, allowed to stand for stratification, and the organic phase is washed with water, dried and rectified to obtain trifluoroisothiocyanate Ethane toluene liquid. used dire...
Embodiment 2
[0022] Embodiment 2: except that the consumption of triethylamine is replaced by 42.9g (1.05eq), all the other are the same as embodiment 1.
[0023] The product yield is 60.7%; the purity is 71.7%, and the purity after deducting toluene is 99.4%.
Embodiment 3
[0024] Embodiment 3: except that triethylamine consumption is replaced by 81.8g (2.0eq), all the other are the same as embodiment 1.
[0025] The yield of the product is 59.4%, the purity is 70.6%, and the purity after deducting toluene is 99.2%.
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Abstract
The invention relates to a preparation method of trifluoroisothiocyanate ethane. The preparation method comprises the steps of 1, mixing trifluoroethylamine, triethylamine and a solvent to obtain a first reaction mixture; controlling the temperature to be 10-12 DEG C, adding carbon disulfide, and reacting at the temperature of 5-20 DEG C to obtain a second reaction mixture containing trifluoroethylamino thioformate, wherein the molar ratio of the trifluoroethylamine to the triethylamine is 1: (1.05-2), the molar ratio of trifluoroethylamine to carbon disulfide is 1: (1-1.2), the molar ratio of trifluoroethylamine to the solvent is 1: (5-8), and the solvent is toluene, xylene or dichloromethane; 2, cooling the second reaction mixture obtained in the step 1 to 5-10 DEG C, adding solid light, stirring at room temperature, heating to the temperature of 35-45 DEG C, and reacting to obtain a trifluoroisothiocyanate ethane mixture; and then cooling, adding water and rectifying to obtain trifluoroisothiocyanate ethane. Compared with the prior art, the method has the advantages of high product yield and less three wastes by adopting solid light as a catalyst. According to the method, toluene / dichloromethane is adopted as the solvent, the problems that tetrahydrofuran and water are mixed and dissolved, part of products are brought into a water phase, the reaction yield is too low, and the solvent is difficult to recover are solved, the solvent can be recovered and reused after being evaporated, the recovery rate reaches 88% or above, the reaction cost is reduced, and emission of three wastes is reduced.
Description
technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of trifluoroisothiocyanate. [0002] technical background [0003] Trifluoroisothiocyanate is a class of important organic synthesis intermediates, widely used in the preparation of organic synthesis products such as pesticides and medicines. In the prior art, the preparation method of trifluoroisothiocyanate generally has problems such as low yield, high cost, and many wastes, and is not suitable for industrial production. Therefore, it is very meaningful to study the preparation route with high yield, low cost and green environmental protection. [0004] There are two main preparation routes of trifluoroisothiocyanate in the prior art, the first route is to use trifluoroethylamine and thiophosgene to react. However, thiophosgene, the raw material for this reaction, is a highly toxic and volatile substance, which is harmful to the environment and ...
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