A kind of synthetic method of tri(diethylamino) tantalum tert-butyramide
A technology of diethylamino and tert-butyramide, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the troublesome synthetic operation process, high cost, low yield, etc. problem, to achieve the effect of high reaction yield and production efficiency, easy to control, and easy to obtain
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0032] A kind of synthetic method of tri(diethylamino) tantalum tert-butyramide, the steps are as follows:
[0033] Step 1) In an argon environment or other inert gas environment, add 150 grams of tantalum pentachloride and 500 milliliters of n-nonane to No. 1 reactor, stir it evenly, and adjust and maintain No. 1 reactor temperature as - 30°C, then add 62 grams of anhydrous tert-butylamine to the No. 1 reactor while stirring, return to room temperature and react for 4 hours after the addition; Add 134 grams of pyridine into the reaction kettle, return to room temperature and react for 4 hours to obtain a mixed solution; filter the mixed solution and concentrate under low pressure to obtain a suspension of tantalum complex.
[0034] Step 2) under argon environment or other inert gas environment, add 510 milliliters of n-butyllithium n-nonane solutions (concentration is 2.5mol / L) in No. 2 reactor, adjust and keep No. 2 reactor temperature as -20°C, and under the condition of s...
Embodiment 2
[0037] A kind of synthetic method of tri(diethylamino) tantalum tert-butyramide, the steps are as follows:
[0038] 1) In an argon environment or other inert gas environment, add 150 grams of tantalum pentachloride and 500 milliliters of n-nonane in the No. 1 reaction kettle, and add 62 grams of anhydrous tert-butylamine into the No. 1 reaction kettle under stirring conditions , keep the temperature at -10°C during the addition, and return to room temperature for 6 hours after the addition; then adjust and maintain the temperature of the No. ; The mixture was filtered and concentrated under low pressure to obtain a suspension of tantalum complexes.
[0039] 2) In an argon environment or other inert gas environment, add 510 milliliters of n-butyllithium n-nonane solution (concentration is 2.5mol / L) in No. Add 95 g of diethylamine dropwise to the kettle, control the rate of dropping and keep the temperature of the solution at -10°C, return to room temperature and react for 5 ho...
Embodiment 3
[0042] In an argon environment or other inert gas environment, add 150 grams of tantalum pentachloride and 500 milliliters of n-nonane in the reaction kettle, and add 62 grams of anhydrous tert-butylamine in the reaction kettle under stirring conditions, and keep the temperature when adding At -15°C, the reaction was resumed at room temperature for 5 hours after the addition, and then 134 g of pyridine was added. During the addition, the temperature of the system was maintained at -15°C, and the reaction was resumed at room temperature for 5 hours after the addition. Filter and concentrate under low pressure to obtain a suspension of tantalum complex.
[0043]Under an argon atmosphere or other inert gas atmosphere, add 510 milliliters of n-butyllithium n-nonane solution (concentration: 2.5mol / L) to the reaction kettle, and add diethyl ether dropwise to the reaction kettle under stirring condition. Amine 95g, control the rate of dropping and keep the temperature of the solution...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More