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ChemicalBook CAS DataBase List 1,4-DIETHYLPIPERAZINE

1,4-DIETHYLPIPERAZINE synthesis

13synthesis methods
-

Yield: 74.4%

Reaction Conditions:

with hydrogen at 200; under 7500.75 - 60006 Torr; for 6 h;Autoclave;Inert atmosphere;

Steps:

1
Example 1 Preparation of N,N'-diethylpiperazine from aminoethylethanol and ethanol The reaction was carried out in a magnetically coupled 300 ml stirring autoclave with electric heating and cascade regulation of the internal temperature.10.4 g of aminoethylethanolamine (IIa1) (0.1 mol), 92 g of ethanol (2 mol) and 10 g of a reduced and passivated catalyst A comprising copper on aluminum oxide (3×3 mm pellets) were introduced into the autoclave which had been made inert by means of nitrogen. The catalyst comprised, before reduction, 55% by weight of copper oxide (CuO) and 45% by weight of aluminum oxide. The reduction was carried out at from 180 to 200° C. and the passivation was carried out at <50° C. using air before the reaction. The reaction mixture was pressurized at room temperature with hydrogen up to a pressure of 10 bar. The autoclave was then heated to 200° C., further hydrogen was injected up to a total pressure of 80 bar and the reaction mixture was stirred (800 rpm) at 200° C. and 80 bar for 6 hours.Gas-chromatographic analysis (GC column 30 m RTX 5 amine) indicated that the reaction output (without excess ethanol) at complete aminoethylethanolamine conversion comprised 74.4% by area of N,N'-diethylpiperazine.

References:

BASF SE US2012/95221, 2012, A1 Location in patent:Page/Page column 8

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