A kind of synthetic method of borohydride anion potassium salt kb3h8
A synthesis method and anion technology, applied in the directions of borane/diborane hydride, etc., can solve problems such as inconvenient operation, and achieve the effect of simple operation
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Embodiment 1
[0020] All manipulations were performed under nitrogen atmosphere. In the glove box, add 0.78 g of potassium metal to a 100 mL schlenk reaction bottle equipped with a magnet, and remove the schlenk reaction bottle from the glove box after sealing with a stopper. Then add a tetrahydrofuran solution (THF•BH) of borane with a molar concentration of 1mol / L 3 ) 40 mL, stirred at room temperature for 8 hours. Remove the insoluble matter by filtration, concentrate the filtrate to remove the solvent to obtain a white sticky solid, then wash the solid with toluene 3 times, 20 mL each time, and then concentrate in vacuo to remove the solvent to obtain a white solid product, which is pure KB without solvent addition. 3 h 8 . The resulting KB 3 h 8 Weighing is 0.64g, the calculated yield is 80%, and its purity is close to 100% in nuclear magnetic detection.
Embodiment 2
[0022] All manipulations were performed under nitrogen atmosphere. In the glove box, add 0.78 g of potassium metal to a 100 mL schlenk reaction bottle equipped with a magnet, and remove the schlenk reaction bottle from the glove box after sealing with a stopper. Then add a tetrahydrofuran solution (THF•BH) of borane with a molar concentration of 1mol / L 3 ) 80mL, stirred and reacted at 0°C for 12 hours. Remove the insoluble matter by filtration, concentrate the filtrate to remove the solvent to obtain a white sticky solid, then wash the solid with toluene 3 times, 20 mL each time, and then concentrate in vacuo to remove the solvent to obtain a white solid product, which is pure KB without solvent addition. 3 h 8 . The resulting KB 3 h 8 Weighing 0.68g, the calculated yield is 85%, and its purity is close to 100% in nuclear magnetic detection.
Embodiment 3
[0024] All manipulations were performed under nitrogen atmosphere. In the glove box, add 0.78 g of potassium metal to a 100 mL schlenk reaction bottle equipped with a magnet, and remove the schlenk reaction bottle from the glove box after sealing with a stopper. Then add a tetrahydrofuran solution (THF·BH) of borane with a molar concentration of 0.5mol / L 3 ) 80 mL, stirred and reacted at room temperature for 10 hours. Remove the insoluble matter by filtration, concentrate the filtrate to remove the solvent to obtain a white sticky solid, then wash the solid with toluene 3 times, 20 mL each time, and then concentrate in vacuo to remove the solvent to obtain a white solid product, which is pure KB without solvent addition. 3 h 8 . The resulting KB 3 h 8 Weighing 0.68g, the calculated yield is 85%, and its purity is close to 100% in nuclear magnetic detection.
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