Potassium Hydroxide → 1-(But-3-yn-1-yl)imidazolidin-2-one

Temperatur

75 °C

To a solution of 1-but-3-ynyl-3-(2-chloro-ethyl)-urea (5 g, 28.7 mmol) in THF (100 mL) add tetrabutylammonium bromide (1.82 g, 5.65 mmol) and potassium hydroxide (2.01 g, 35.9 mmol). Heat the resulting suspension at 75° C. for 72 h and allow to cool to room temperature. Dilute the mixture with EtOAc (200 mL), wash with water (2×100 mL) and 1N aqueous HCl (100 mL). Dry the organic phase over MgSO4, filter and concentrate in vacuo to obtain the title compound as a white powder (816 mg, 21%).

1. temperatureto cool to room temperature
2. washwash with water (2×100 mL) and 1N aqueous HCl (100 mL)
3. dry with materialDry the organic phase over MgSO4
4. filtrationfilter
5. concentrationconcentrate in vacuo

ORD-Eintrag

ord-4cac3a6b517f48ecaaef63dc16fd2ff4

Quelldatensatz

uspto-grants-2013_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08420631B2