Production of methy borate alkane tetrahydrofuran complex solution
A technology of tetrahydrofuran and complex compound is applied in the field of preparation of borohydride reagent borane tetrahydrofuran complex solution, and can solve the problems of high price of sodium borohydride, slow speed of borane tetrahydrofuran complex, and expensive manufacturing cost of borane and other problems, to achieve the effect of simple and convenient process operation, low cost and reduced equipment requirements
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Embodiment 1
[0017] In a 1000 ml three-neck flask with mechanical stirring and a thermometer, add 500 ml of tetrahydrofuran, 54 g of 98.5% potassium borohydride (1.0 mole) and 42 g of anhydrous lithium chloride (1.0 mole), fill with nitrogen and stir vigorously The temperature was raised to reflux, and the reaction was carried out under reflux at 67° C. for 10 hours, and the stirring speed was kept at 800 rpm. After the reaction is completed, cool to 0°C under a nitrogen atmosphere, add 189 grams of boron trifluoride etherate complex dropwise at this temperature, and continue stirring for 1 hour. After the reaction is completed, filter it with a filter stick under nitrogen pressure, and the filter residue is an inorganic salt. , add tetrahydrofuran to fully wash the filter residue until the filtrate is exactly 1000 ml. The concentration of borane was determined to be 1.26M, and the yield was 94.5%.
Embodiment 2
[0019] In a 1000 ml three-neck flask with mechanical stirring and a thermometer, add 500 ml of tetrahydrofuran, 54 g of 98.5% potassium borohydride (1.0 mol) and 42 g of anhydrous lithium chloride (1.0 mol), fill with nitrogen and stir vigorously The temperature was raised to reflux, and the reaction was carried out under reflux at 67°C for 18 hours, and the stirring speed was kept at 300 rpm. After the reaction is completed, cool to 0°C under a nitrogen atmosphere, add 189 grams of boron trifluoride etherate complex dropwise at this temperature, and continue stirring for 1 hour. After the reaction is completed, filter it with a filter stick under nitrogen pressure, and the filter residue is an inorganic salt. , add tetrahydrofuran to fully wash the filter residue until the filtrate is exactly 1000 ml. The concentration of borane was determined to be 1.05M, and the yield was 78.8%.
Embodiment 3
[0021] In a 1000 ml three-neck flask with mechanical stirring and a thermometer, add 500 ml of tetrahydrofuran, 54 g of 98.5% potassium borohydride (1.0 mol) and 42 g of anhydrous lithium chloride (1.0 mol), fill with nitrogen and stir vigorously The temperature was raised to reflux, and the reaction was carried out under reflux at 67° C. for 10 hours, and the stirring speed was kept at 800 rpm. After the reaction is completed, cool to 20°C under a nitrogen atmosphere, add 189 grams of boron trifluoride etherate complex dropwise at this temperature, and continue stirring for 1 hour. After the reaction is completed, filter it with a filter stick under nitrogen pressure, and the filter residue is an inorganic salt , add tetrahydrofuran to fully wash the filter residue until the filtrate is exactly 1000 ml. The concentration of borane was determined to be 1.24M, and the yield was 93.0%.
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