2-Amino-2-methyl-1-propanol → 2,2,5,5-tetramethylpiperazine

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Reaction Steps

In this example, 139 cc of a Ni-Fe-Cu-Mn catalyst (1/8" diameter) were charged to an 0.815" ID tubular upward flow reactor. A liquid feed containing 2-amino-2-methyl-1-propanol and tetraglyme (a tetraethylene glycol dimethyl ether solvent) (1/1.18 by weight) was pumped through the catalyst bed at a rate of 0.12 lb/hr at 240° C. Hydrogen was also passed through the reactor at a rate of about 6 L/hr. The pressure was maintained at 800 psig. The products were collected. GLC analysis showed that a 62% yield of 2,2,5,5-tetramethylpiperazine and a 14% yield of 3,3,6,6-tetramethyl-2-piperazinone were obtained with a 90% conversion of 2-amino-2-methyl-1-propanol. The resulting reaction mixture was fractionally distilled at atmospheric pressure under nitrogen. Both products were further recrystallized from ether.

Provenance & Evidence