Ethylenediamine → Piperazine,2-(3-methoxy-4-nitrophenyl)-

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Reaction Steps

(RS)-2-(3-Methoxy-4-nitrophenyl)piperazine was prepared according to the method described in Patent Application FR 2,351,108, but starting with 3-methoxy-4-nitrophenylglyoxal (36 g) and ethylenediamine (12.1 g). The crude product is purified by chromatography on 230-400 mesh silica (800 g) suspended in a mixture of dichloromethane (70%), ethanol (26%) and triethylamine (4%) and elution with the same mixture (2 liters). After concentration of the eluate under reduced pressure (20 kPa) at approximately 50° C., the expected product (18 g) is obtained in the form of a red oil, which was used without further purification for the subsequent steps.

Provenance & Evidence