Sodium Carbonate → 1-(Tetrahydro-2-furoyl)piperazine

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Reaction Steps

The furoylpiperazine of Example 1 was converted to the hydrobromide salt (m.p. 173°-175° C). This salt (39.0 g) in 250 ml methyl alcohol and 9.0 g Raney nickel was hydrogenated at 3 atm. After uptake of H2 ceased, the catalyst was filtered, the solvent concentrated, and the residue crystallized from isopropyl alcohol to give 35.2 g. tetrahydrofuroylpiperazine HBr, m.p. 152°-156 ° C. This was suspended in 20 ml H2O. Then 10.5 g 50%, NaOH solution was added slowly followed by 2.0 g solid Na2CO3. This was extracted with 4×100 ml portions of warm CHCl3. The CHCl3 extractions were distilled to give 22.5 g tetrahydrofuroylpiperazine, b.p. 120°-125° C./0.2 mmHg.

Provenance & Evidence