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ChemicalBook CAS DataBase List Piperazine

Piperazine synthesis

15synthesis methods
Piperazine (38.1.12) is a bulk product in organic synthesis. It is made from ethanolamine by heating it in ammonia at a temperature of 150–220°C and a pressure of 100–250atm. It is used as a drug in the form of a salt, and as a rule, in the form of adipinate.

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Yield:111-40-0 97.53% ,110-85-0 1.03%

Reaction Conditions:

with ammonia;hydrogen;potassium hydroxide in ethanol at 80; under 90009 Torr;Pressure;Reagent/catalyst;Solvent;Temperature;Time;

Steps:

5

The anion exchange resin (available from Dandong Mingzhu Special Type Resin Co., LTD, D202) was treated according to the same process of transformation as in Example 1. In 1L stainless high-pressure reactor were added the mixture of 12 g of the transformed resin, 10 g of the cesium acetate treated molecular sieve of Y type (H_=37, produced by impregnating the molecular sieve powder of Na-Y type (Wenzhou Catalyst Plant) with 1.2 mol/L cesium acetate solution at a solid-to-liquid ratio of 1:10 for 5 times at 65°C, calcining for 5 hours at 650°C after drying at 120°C, and cooling in a dryer), 30 g Raney cobalt (available from Süd-Chemie AG, German, ACTICA3100), 60 g IDAN and 400 ml ethanol. Then 7.6 ml of 5% KOH ethanol solution was added. The atmosphere of the reaction system was exchanged by N2. After 34 g of liquid ammonia was added into the reaction system which was heated while stirring, H2 was introduced into the reactor. The reaction was performed at the temperature of 80°C and under the pressure of 12 Mpa. After the reaction was completed, the solution was collected and analyzed by GC. The conversion of IDAN was 100%, the selectivity of DETA was 97.53%, and the selectivity of piperazine was 1.03%.

References:

EP2684862,2014,A1 Location in patent:Paragraph 0041

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