Piperazine → 1-Butylpiperazine

Anhydrous piperazine (19.5 g) was dissolved in ethanol (100 ml), and a solution of 1-bromobutane (24.8 g) in ethanol (50 ml) was added dropwise over a period of 20 minutes at room temperature. After stirring overnight, the reaction solution was filtered off with Celite, and the solvent was distilled off under reduced pressure. To the residue obtained was added a 40% aqueous solution of sodium hydroxide, and extracted with ether three times. The ether layer was dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (methylene chloride:methanol:aqueous ammonia=90:10:0.5) to give the title compound (7.53 g) as a yellow oily substance. Yield=29%.

1. filtrationthe reaction solution was filtered off with Celite
2. distillationthe solvent was distilled off under reduced pressure
3. customTo the residue obtained
4. extractionextracted with ether three times
5. dry with materialThe ether layer was dried over anhydrous magnesium sulfate
6. distillationthe solvent was distilled off under reduced pressure
7. customThe residue was purified by silica gel column chromatography (methylene chloride:methanol:aqueous ammonia=90:10:0.5)

ORD record

ord-ce09ba1a1cb34bdeae8b1aa6ed715b94

Source dataset

uspto-grants-1999_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05945434