Potassium Carbonate → Tert-butyl 4-(but-3-yn-1-yl)piperazine-1-carboxylate

Temperatur

60 °C

To a solution of 1-Boc-piperazine (0.5 g, 2.68 mmol) in acetonitrile (2.5 mL) was added K2CO3 (0.55 g, 4.02 mmol) followed by 4-bromo-1-butyne (0.39 g, 2.95 mmol). The mixture was heated at 60° C. for 6 h, allowed to come to room temperature, diluted with water and extracted with EtOAc (2×15 mL). The combined organic layers washed with water, brine, dried over Na2SO4 and concentrated under vacuo to afford the title compound (0.55 g, 86%); LCMS: m/z=239.10 (M+1). Method 2minLowp.

1. customto come to room temperature
2. extractionextracted with EtOAc (2×15 mL)
3. washThe combined organic layers washed with water, brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated under vacuo

ORD-Eintrag

ord-73850401e58f425daf9602b359bfec31

Quelldatensatz

uspto-grants-2015_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09174978B2