Process for producing tertiary butylamine ethoxy ethyl alcohol with space steric effect
A technology of tert-butylaminoethoxyethanol and steric hindrance effect, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxyl compounds, etc., which can solve the problem of large volatilization loss, increased purification cost, and reduced economic benefits and other problems, to achieve the effect of high solvent boiling point, saving operating costs, and high purification efficiency
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Embodiment 1
[0012] A. 2 liters of ethanol with a purity of 97%, 657g of tert-butylamine with a content of 95%≥, and 450g of 2-chloroethoxyethanol are put into the reactor, heated to 100-120°C, and reacted under self-pressure for 2.0 hours;
[0013] B. After cooling the above reactant to 60°C, add 220g of KOH with a content of 95%, and neutralize it under reflux for 1.0 hour, then cool to ≤30°C to recover excess tert-butylamine;
[0014] C, the filtrate after above-mentioned solution filtration is placed in crude distillation under 160 ℃ of temperature and 0.03MPa vacuum;
[0015] D. After rectifying the crude distillate obtained from C at a temperature of 190° C. and a vacuum condition of 0.03 MPa, 442 g of a tert-butylaminoethoxyethanol product was obtained. The content of this product was 95.8% through chromatographic analysis.
Embodiment 2
[0017] The processing steps of this embodiment are the same as those of Embodiment 1.
[0018] First, mix 91g of tert-butylamine of industrial purity, 62g of 2-chloroethoxyethanol and 200ml (milliliters) of methanol into a 600-liter reactor, and react under pressure at 145°C for 1.5 hours, then cool to about 50°C, and then Add 22g of NaOH with a content of 98% and neutralize under reflux for 1.0 hour, then cool to about 25°C to recover excess tert-butylamine; then filter, reduce pressure, crude distillation and rectification to obtain tert-butylaminoethoxy Ethanol product 62g, product content 95.6%.
Embodiment 3
[0020] In this embodiment, water is used as the reaction medium, 46g of tert-butylamine, 31g of 2-chloroethoxyethanol (both industrially pure) and 30ml of water are mixed, placed in a steel reaction kettle, the reaction temperature is 160°C, and the pressure is 0.6-0.7MPa After reacting for 50 minutes, cool down to 65°C together with the reactor, then add 11g of 98% NaOH for neutralization treatment for 45 minutes, lower the temperature to room temperature (about 28°C) and recover excess tert-butylamine, then filter the reactant; The filtrate was crudely distilled at a temperature of 170°C and a pressure of 0.04MPa; the distillate was further rectified at a temperature of 190°C and a pressure of 0.04MPa to obtain 33g of a product with a content of 98.1%. In this embodiment, the reaction speed is fast, the effect is good, the medium does not need to be recycled, and the technical and economic benefits are obvious.
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