Method for preparing potassium trifluoroborate series compounds

Abstract

The invention relates to synthesis of organic compounds, and provides a method for preparing potassium trifluoroborate series compounds. The method comprises the following steps of: adding organic boric acid or organic borate and solvent (THF (tetrahydrofuran), or MTBE (Methyl Tertiary Butyl Ether), or ethyl acetate, or methanol) into a reaction kettle lined with tetrafluoroethylene plastic at room temperature; adding potassium bifluoride and water at normal temperature, stirring for 1 to 12 hours, and reacting to prepare a solid-liquid mixture; adding solid potassium ion containing inorganic or organic alkali into the solid-liquid mixture after the reaction is completed, neutralizing until the pH is between 7 and 9, and continuously stirring for 1 to 5 hours; directly filtering to obtain a solid coarse product after stirring is completed; dissolving the coarse product with solvent, filtering and concentrating, adding nonpolar solvent, and pulping to obtain high-quality RBF3K series compounds. The method is easy to operate, has mild reaction conditions, and can realize scale-up production; and the product prepared by the method has high yield and excellent purity, and the cost is greatly reduced.

Description

technical field [0001] The present invention relates to the synthesis method of organic compound, especially the synthesis method of potassium trifluoroborate compound. Background technique [0002] Potassium trifluoroborate series compounds are widely used by drug developers because of their stable structure, convenient transportation and storage, and long-term storage. In the literature, the synthesis of potassium trifluoroborate series compounds generally uses the organic solution of organic boric acid or borate to react with the aqueous solution of potassium bifluoride, and then evaporates the solvent and water under high vacuum, and the obtained crude product is either dissolved in acetone and removed by filtration. Impurities were purified, or the desired product was eluted with acetone by Soxhlet extraction. The acetone solution is then crystallized by ether, MTBE, THF and other solvents to obtain a white crystal product. [0003] From the reaction equation and proc...

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Problems solved by technology

[0003] From the reaction equation and process description, this method is simple and feasible, but in the actual production process, there are many defects in this method, and it cannot even be enlarged; the first, the raw material potassium bifluoride produces hydrofluoric acid in the reaction process, and this material has Extremely corrosive, relatively special to equipment requirement, and literature method does not propose solution; Second, this literature method mentions underpressure distillation under high vacuum to remove water, because it is a one-pot synthesis, produces a large amount of In production, it is difficult to distill the water clean. Third, the process produces KF during the reaction process, and it is easy to form dihydrate with water, and the crystal water cannot be removed under the process conditions. After dissolving in acetone in the presence of water, there will be two problems: a. The material is acidic and cannot be separated by metal or enamel equipment; b. Dissolving in acetone in the presence of water, inorganic salts are It is difficult to remove, it is difficult to obtain high-quality products; such a method is difficult to carry out in production, and it is unsafe; in summary, the preparation of potassium trifluoroborate series compounds by the method of this document is not suitable scaled up mass production

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