Water → 2-[4-(5-Bromopyrimidin-2-yl)piperazin-1-yl]ethanol

To a solution of 5-bromo-2-(piperazin-1-yl)pyrimidine (0.20 g, 0.83 mmol) in acetone (10.0 mL) was added K2CO3 (0.58 g, 4.17 mmol) followed by the addition of 2-bromoethanol (0.01 g, 1.66 mmol). The resulting reaction mixture was heated to reflux for 3 h. After the completion of reaction (TLC monitoring), the reaction mixture was cooled, added water and extracted with EtOAc (2×100 mL). The combined organics was washed with brine, dried (Na2SO4), filtered and concentrated. The crude residue was purified over silica gel (100-200 M, 2% MeOH-DCM) to obtain the desired product (0.11 g, 47%). MS: 287.10 (M+H)+.

1. customThe resulting reaction mixture
2. temperaturewas heated
3. temperatureto reflux for 3 h
4. customAfter the completion of reaction (TLC monitoring)
5. temperaturethe reaction mixture was cooled
6. extractionextracted with EtOAc (2×100 mL)
7. washThe combined organics was washed with brine
8. dry with materialdried (Na2SO4)
9. filtrationfiltered
10. concentrationconcentrated
11. customThe crude residue was purified over silica gel (100-200 M, 2% MeOH-DCM)

ORD-Eintrag

ord-a44aee34b83146059c61ecf224e6bc30

Quelldatensatz

uspto-grants-2012_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08299065B2