The method of synthesizing n,n-diisopropylethylamine
A technology of diisopropylethylamine and diisopropylamine, which is applied in the field of synthesizing N,N-diisopropylethylamine, can solve the problems of high bromoethane price, high use cost, and poor safety, and achieve post-processing The effect of simplicity, low cost of raw materials, and convenient operation
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Embodiment 1
[0018] Embodiment 1, a kind of synthetic method of DIPEA, carry out following steps successively:
[0019] Add 101.1g (1.0mol) diisopropylamine, 332.0g (2.0mol) tetraethylammonium chloride, 101.1g ethanol, 60g (1.5mol) sodium hydroxide to a 1000ml three-necked flask, heat to reflux, and keep The reaction at the reflux temperature (80°C) was completed after 7 hours, cooled to room temperature, and the reaction mixture was removed from the solvent on a rotary evaporator, then washed with 200mL*3 deionized water, and the oil phases washed three times were combined and collected directly under normal pressure. After rectification, 124.1 g of fractions at 125-127°C were collected, which was the product DIPEA, with a yield of 96.2% and a purity of 99.5% as detected by gas chromatography.
[0020] Remarks: The reactant is a solid-liquid mixture after removing low boilers and cooling to room temperature, and becomes a water-oil two-phase after washing.
Embodiment 2
[0021] Embodiment 2: a kind of synthetic method of DIPEA, carries out following steps successively:
[0022] Add 101.1g (1.0mol) of diisopropylamine, 166.0g (1.0mol) of tetraethylammonium chloride, 151.7g of n-propanol, and 106g (1.0mol) of sodium carbonate into a 1000ml three-necked flask, heat to reflux, and Keep the reflux temperature (98°C) for 5 hours and finish the reaction, cool to room temperature, remove the solvent from the reaction mixture on a rotary evaporator, wash with 200mL*3 deionized water, combine and collect the oil phases washed three times and directly normalize Pressure rectification collected 124.4 g of fractions at 125-127° C., which was the product DIPEA, with a yield of 96.4% and a purity of 99.5% as detected by gas chromatography.
[0023] Remarks: The reactant is a solid-liquid mixture after removing low boilers and cooling to room temperature, and becomes a water-oil two-phase after washing.
Embodiment 3
[0024] Embodiment 3: a kind of synthetic method of DIPEA, carries out following steps successively:
[0025] Add 101.1g (1.0mol) of diisopropylamine, 210.2g (1.0mol) of tetraethylammonium bromide, 202.2g of isopropanol, and 138g (1.0mol) of potassium carbonate to a 1000ml three-necked flask, and maintain the reflux temperature (82°C) After 3 hours of reaction, it was cooled to room temperature, and the reaction mixture was removed from low boilers on a rotary evaporator, washed with 200mL*3 deionized water, and the oil phases washed three times were combined and directly purified under normal pressure. Distillation, collecting 121.2 g of fractions at 125-127 ° C, which is the product DIPEA, the yield is 94.0%, and the purity detected by gas chromatography is 99.6%.
[0026] Remarks: After the reactant removes the low boiling matter and cools to room temperature, it becomes a solid-liquid mixture. After washing, the solid sodium chloride and quaternary ammonium salt are dissolv...
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