Background and overview of the preparation method of boron trifluoride tetrahydrofuran complex
Boron trifluoride tetrahydrofuran complex is a catalyst for the preparation of a variety of pharmaceutical products (such as cephalosporins, methoxyphenylboronic acids, and floxacin). It is also an important raw material for the preparation of borane and targeted drugs. The traditional production method of this product is to add tetrahydrofuran to the reaction tank, pass boron trifluoride gas into the tetrahydrofuran liquid during the cooling process to form a boron trifluoride complex, and then distill it to remove the color to obtain the finished product.
Preparation method of boron trifluoride tetrahydrofuran complex
Report on the preparation method of boron trifluoride tetrahydrofuran complex 1.
CN202010573013.3 provides a preparation method of boron trifluoride tetrahydrofuran complex. The preparation method can instantly complex tetrahydrofuran and boron trifluoride, and can avoid oxidation and discoloration of tetrahydrofuran under vacuum conditions, and adopts independent The desulfurization process eliminates the distillation desulfurization process and reduces the water content and sulfur dioxide content in the product.
Use the first vacuum pump 2, the second vacuum pump 12 and the third vacuum pump 17 to respectively evacuate the tetrahydrofuran vaporization tank 6, the reaction tank 13 and the desulfurization tank 21 to -0.1MPa and keep it for 1 hour;
Under stirring (80 rpm) conditions, add 50kg tetrahydrofuran into the tetrahydrofuran vaporization tank 6 and heat the tetrahydrofuran in the tetrahydrofuran vaporization tank 6 through the first steam heating device, and maintain the temperature of the tetrahydrofuran at 80℃, and reach the gas-liquid equilibrium state (0.15MPa);
Pour in cold water through the cold water inlet 9, pass the tetrahydrofuran vapor at a rate of 25kg/h, and the boron trifluoride vapor at a rate of 23.61kg/h into the reaction tank 13 to start the complexing reaction. After the reaction is completed, the reaction solution The temperature is 80°C, and it is cooled to 50°C under stirring (80 rpm) conditions to obtain crude boron trifluoride tetrahydrofuran complex;
Transport the crude boron trifluoride tetrahydrofuran complex dihydroxypyridine hydrochloride into the desulfurization tank, and maintain vacuum (-0.1MPa) conditions under stirring (80 rpm) conditions, and pass The second steam heating device heats to 50°C and maintains it for 3 hours. After desulfurization, the temperature is lowered to 25°C and the material is discharged to obtain the boron trifluoride tetrahydrofuran.
Preparation method report of boron trifluoride tetrahydrofuran complex 2.
The production process of boron trifluoride tetrahydrofuran includes the following steps:
Slowly drop tetrahydrofuran into the caustic soda kettle, absorb water to generate tetrahydrofuran vapor, introduce tetrahydrofuran vapor into the complexing device, and at the same time introduce boron trifluoride gas for complexation reaction. According to the ratio between tetrahydrofuran and boron trifluoride gas The reaction was carried out at a mass ratio of 1:2, the temperature was controlled between 30°, and the reaction time was 2 hours; after drying, boron trifluoride tetrahydrofuran was obtained.
References
[1] CN202010573013.3 Preparation method of boron trifluoride tetrahydrofuran complex
[2] CN201210424080.4 Preparation method of boron trifluoride tetrahydrofuran
