Synthesis method of boron hydride [NH3BH2NH3]B3H8
A technology of borohydride compounds and synthesis methods, which is applied in the field of synthesis of borohydride compounds, can solve problems such as cumbersome synthesis steps, and achieve the effect of simple operation
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Embodiment 1
[0016] All manipulations were performed under nitrogen atmosphere. In the glove box, add 0.31 g of ammonia borane to the 100 mL schlenk reaction bottle equipped with a magnet, seal the schlenk reaction bottle with a stopper, and then remove the schlenk reaction bottle from the glove box, and then add 50 mL of B with a molar concentration of 0.1 mol / L 3 h 7 Tetrahydrofuran solution in THF·B 3 h 7 , stirred at room temperature for 8 hours, filtered to remove insoluble matter, concentrated the filtrate to remove the solvent to obtain a white sticky solid, then washed the solid with toluene 3 times, 20 mL each time, then concentrated in vacuo to remove the solvent to obtain a white solid product, which is borohydride [ NH 3 BH 2 NH 3 ]B 3 h 8 , the resulting [NH 3 BH 2 NH 3 ]B 3 h 8 Weighing 0.36g, the calculated yield is 82%, and its purity is close to 100% in nuclear magnetic detection.
Embodiment 2
[0018] All manipulations were performed under nitrogen atmosphere. In the glove box, add 0.31 g of ammonia borane to a 100 mL schlenk reaction bottle equipped with a magnet, seal the schlenk reaction bottle with a stopper, then remove the schlenk reaction bottle from the glove box, and then add 5 mL of B with a molar concentration of 1 mol / L 3 h 7 Tetrahydrofuran solution in THF·B 3 h 7, stirred at 0°C for 12 hours, filtered to remove insoluble matter, concentrated the filtrate to remove the solvent to obtain a white sticky solid, then washed the solid with toluene 3 times, 20 mL each time, then concentrated in vacuo to remove the solvent to obtain a white solid product, which is borohydride [NH 3 BH 2 NH 3 ]B 3 h 8 , the resulting [NH 3 BH 2 NH 3 ]B 3 h 8 Weighing is 0.35g, the calculated yield is 80%, and its purity is close to 100% in nuclear magnetic detection.
Embodiment 3
[0020] All manipulations were performed under nitrogen atmosphere. In the glove box, add 0.15 g of ammonia borane to a 100 mL schlenk reaction bottle equipped with a magnet, seal the schlenk reaction bottle with a stopper, and then remove the schlenk reaction bottle from the glove box, and then add 10 mL of B with a molar concentration of 0.5 mol / L 3 h 7 Tetrahydrofuran solution in THF·B 3 h 7 , stirred at room temperature for 6 h, filtered to remove insoluble matter, concentrated the filtrate to remove the solvent to obtain a white sticky solid, then washed the solid with toluene 3 times, 20 mL each time, then concentrated in vacuo to remove the solvent to obtain a white solid product, which is borohydride [ NH 3 BH 2 NH 3 ]B 3 h 8 , the resulting [NH 3 BH 2 NH 3 ]B 3 h 8 Weighing 0.36g, the calculated yield is 82%, and its purity is close to 100% in nuclear magnetic detection.
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