- Preparation method of trifluoroisothiocyanate ethane
-
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.
- -
-
Paragraph 0019-0114
(2021/06/23)
-
- AZOLE COMPOUNDS AS PIM INHIBITORS
-
The invention relates to bicyclic compounds of formulas I and Ia, and salts thereof. In some embodiments, the invention relates to inhibitors or modulators of Pim-1 and/or Pim-2, and/or Pim-3 protein kinase activity or enzyme function. In still further em
- -
-
Page/Page column 162
(2012/10/08)
-