A kind of preparation method of pinacol borane
A technology of pinacol borane and dichloroborane is applied in the field of preparation of pinacol borane, can solve the problems of high cost of borane and high market price of pinacol borane, and achieves simple synthesis method and cheap raw materials , the effect of reducing production costs
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[0025] The preparation method of pinacol borane provided by the invention comprises carrying out condensation reaction with pinacol and dichloroborane under alkaline conditions, and its specific reaction process is as follows:
[0026]
[0027] According to the preparation method of pinacol borane provided by the present invention, the alkaline condition is usually controlled by adding an organic base to the reaction system.
[0028] The present invention is not particularly limited to the amount of dichloroborane, pinacol and organic base, as long as the condensation reaction product with pinacol borane as the main product can be obtained, preferably, the dichloroborane The molar ratio of alkane, pinacol and organic base is 1:1-1.5:2-4, more preferably 1:1-1.3:2-3, especially preferably 1:1-1.2:2-2.5.
[0029] The organic base can be various existing basic organic compounds, and its specific examples include but not limited to triethylamine, diisopropylethylamine, N,N-diet...
Embodiment 1
[0040] This embodiment is used to illustrate the preparation method of pinacol borane provided by the invention.
[0041] Add 100mL of dichloromethane to a 500mL four-neck round bottom flask under nitrogen protection, add 100mL of dichloroborane in dioxane solution (1.0mol / L) at 0°C, and then add 11.82g (0.1mol) of dichloromethane 20.24g (0.2mol) of triethylamine was added dropwise to 20.24g (0.2mol) of triethylamine, the pH value of the reaction system was 11 after the drop, and then the temperature was raised to 20°C and stirred for 12 hours. The solid was filtered out under the protection of nitrogen, and the filtrate was rectified under reduced pressure to obtain 11.25g pinacol borane, yield is 88%, its 1 H NMR spectrum as figure 1 shown, from figure 1 It can be seen that the nuclear magnetic signal at the chemical shift of 1.273ppm is the four methyl signals of the product pinacol borane. It can be seen that the product prepared by the above method is indeed pinacol bo...
Embodiment 2
[0043] This embodiment is used to illustrate the preparation method of pinacol borane provided by the invention.
[0044]Add 100mL of dichloromethane to a 500mL four-necked round bottom flask under nitrogen protection, add 100mL of dichloroborane in dioxane solution (1.0mol / L) at 0°C, and then add 15.37g (0.13mol) of dichloromethane Nacohol, add 38.77g (0.3mol) diisopropylethylamine dropwise, the pH value of the reaction system after the drop is 11, then raise the temperature to 20°C and stir the reaction for 12h, filter the solid under the protection of nitrogen, and depressurize the filtrate Rectification obtains 11.45g of pinacol borane, and the yield is 89%.
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