2-Bromoethanol → 2-[4-(2-Fluoroethyl)piperazin-1-YL]ethanol

1-(2-Fluoroethyl)piperazine diTFA salt (464 mg, 1.29 mmol), (prepared as described for the starting material in Example 27), was dissolved in acetonitrile (3.5 ml). Potassium carbonate (889 mg, 6.44 mmol) and 2-bromoethanol (95 μl, 1.34 mmol) were added and the mixture heated to 85° C. and left overnight. More bromoethanol (95 μl, 1.34 mmol) was added and the reaction mixture heated at 85° C. for a further 2 hours. The reaction mixture was cooled, filtered and concentrated. The residue was purified by column chromatography eluting with methylene chloride/methanol (saturated with ammonia) (92/8) to give 2-[4-(2-fluoroethyl)piperazin-1-yl]ethanol (151 mg, 66%).

1. temperaturethe reaction mixture heated at 85° C. for a further 2 hours
2. temperatureThe reaction mixture was cooled
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was purified by column chromatography
6. washeluting with methylene chloride/methanol (saturated with ammonia) (92/8)

ORD 기록

ord-5265d32b002a4d96ad1c6bf20aa83d17

출처 데이터셋

uspto-grants-2012_10

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08293902B2