1-(2-Hydroxyethyl)piperazine → 4-Butyl-1-piperazineethanol

2-(1-Piperazinyl)ethanol (12.2 g) was dissolved in chloroform (60 ml), triethylamine (13.0 ml) and 1-bromobutane (14.1 g) were successively added at room temperature, and the mixture was stirred overnight. The reaction solution was successively washed with a 10 M aqueous solution of potassium hydroxide (15 ml), water (50 ml×2), saturated aqueous sodium chloride (50 ml), dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue obtained was purified by silica gel column chromatography (methylene chloride:methanol:aqueous ammonia=90:10:0.5) to give the title compound (10.8 g) as a pale yellow oily substance. Yield=62%.

1. washThe reaction solution was successively washed with a 10 M aqueous solution of potassium hydroxide (15 ml), water (50 ml×2), saturated aqueous sodium chloride (50 ml)
2. dry with materialdried over anhydrous magnesium sulfate
3. distillationthe solvent was distilled off under reduced pressure
4. customThe residue obtained
5. customwas purified by silica gel column chromatography (methylene chloride:methanol:aqueous ammonia=90:10:0.5)

ORD record

ord-4440e070be8f45d3bff7f5bf1ef3e5eb

Source dataset

uspto-grants-1999_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05945434