Method for preparing potassium trifluoroborate series compounds

A technology of potassium trifluoroborate and compound, applied in the field of synthesis of potassium trifluoroborate compound, can solve the problem that potassium trifluoroborate series compounds are not suitable for large-scale production, the literature method does not propose a solution, and it is difficult to obtain high-quality products and other problems, to achieve the effect of excellent purity, simplified operation and easy operation

Inactive Publication Date: 2011-05-18
大连联化医药技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Method used

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  • Method for preparing potassium trifluoroborate series compounds
  • Method for preparing potassium trifluoroborate series compounds
  • Method for preparing potassium trifluoroborate series compounds

Examples

Experimental program
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Effect test

Embodiment 1

[0019]

[0020] At room temperature, a 500ml glass four-necked flask is equipped with mechanical stirring, a low temperature thermometer, a 200ml constant pressure dropping funnel, and an argon system; add 25g of dibromomethane, 27.05g of triisopropyl borate, and 200g of THF, and start stirring; Cool down with acetone dry ice freezing liquid; maintain the temperature of the kettle at -78°C, add 41.08g of n-butyllithium solution (2.5M / L) dropwise for about 2~4 hours; after the addition, keep the temperature of the kettle at -70~-78 Incubate at ℃ for 2-4 hours, quench with sulfuric acid aqueous solution, the reaction is completed, add 10% sulfuric acid aqueous solution dropwise to the reaction kettle to quench, adjust PH = 0 to 3; static layer, separate the water layer and extract with MTBE, the organic layer Put it into a 500ml four-necked bottle after merging, start stirring; add 44.94g KHF2 solid, 25g water, maintain the temperature of the kettle at 0-35°C, keep stirring...

Embodiment 2

[0022]

[0023] At a temperature of about 10-35°C, the Grignard reaction is initiated. Put 0.12mol of fluorobromobenzene (dissolved in 80mL ether) into a 500ml glass four-neck flask, and the amount of magnesium used is 1~1.5eq; slowly add the reaction solution dropwise to 0.26mol of B(OR)3 in ether solution Control the temperature at -70~-78°C; after the dropwise addition, control the temperature at about 0°C, add 10mL of 15% hydrochloric acid to adjust the pH value to about 1~2; separate the organic layer, and extract once with an equal amount of THF. The organic layers were combined, dried, the solvent was distilled off under reduced pressure, and beaten with diethyl ether to obtain 13.10 g of fluorophenylboronic acid, with a yield of 78%.

[0024] Dissolve 12.6 grams of fluorophenylboronic acid in 35 mL of methanol, add 25 grams of potassium bifluoride and 20 grams of water, after the addition is complete, stir for 3 to 12 hours; add K2CO3 to neutralize to pH = 7 to...

Embodiment 3

[0027]

[0028] Add 6.6g of 2-trifluoromethylfuran (0.0487mol) to a dry 100mL four-neck flask equipped with mechanical stirring and protected by argon (nitrogen is also acceptable) placed in a freezer, and 32ml of tetrahydrofuran is stirred to cool down ; Add n-butyllithium (19ml / 2.5M, 0.0485mol) dropwise to the reaction flask at 10~-18°C, after the addition is complete, keep it at -5~10°C for 1~3h; cool down to -72°C, and control it at -65℃~-78℃, start to add triisopropyl borate (13.8g, 0.073mol, 1.5eq) dropwise, keep warm for 2h after the dropwise addition; add 10ml MTBE to the reaction system, control the temperature below 15℃, add under stirring 1N HCl pH=6~7;

[0029] The aqueous layer was extracted with MTBE, the organic layers were combined, 11.4g of potassium bifluoride (0.146mol) and 4.2g of water were added under stirring at room temperature, and after stirring for 2-12 hours, potassium carbonate was added to adjust the pH to 7-9 and stirred for 1-3 , filtered, a...

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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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02
Inventor 杨兆辉
Owner 大连联化医药技术有限公司
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