Potassium Carbonate → 5-bromo-1-(2-methoxyethyl)pyridin-2(1H)-one

To a solution of 5-bromo-2(1H)-pyridone (0.10 g, 0.57 mmol) in acetone (5.0 ml) was added K2CO3 (0.18 g, 2.60 mmol followed by addition of 2-bromo-ethyl-methylether (0.24 g, 1.70 mmol). The resulting reaction mixture was heated to 60° C. for 16 h. After the completion of reaction (TLC monitoring), acetone was distilled off, added water and extracted with DCM (3×10 mL). The combined organics was washed with brine, dried (Na2SO4), filtered and concentrated. The crude residue was purified over silica gel (60-120 M, 1% MeOH-DCM) to obtain the desired product (0.10 g, 75%). MS: 232.01 (M+H)+.

1. customThe resulting reaction mixture
2. distillationwas distilled off
3. additionadded water
4. extractionextracted with DCM (3×10 mL)
5. washThe combined organics was washed with brine
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated
9. customThe crude residue was purified over silica gel (60-120 M, 1% MeOH-DCM)

ORD-Eintrag

ord-f66bc8bd6ec247fa84a6a387bb7a5ee9

Quelldatensatz

uspto-grants-2012_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08299065B2