Isopropyl iodide → 4-(1-Methylethyl)morpholine-3-carboxamide

Temperatur

150 °C

To a solution of 1.1 g (6.3 mmol) of morpholine-3-carboxamide (a synthesis of which is described in WO-2005/026 156, Hennequin L. F. A. et al.) in acetonitrile (16 ml) are successively added 1.86 g (22.2 mmol) of sodium hydrogen carbonate powder and 0.7 ml (7.0 mmol) of isopropyl iodide, and the mixture is then heated at 150° C. by microwave for 30 minutes. The reaction mixture is cooled to room temperature, diluted with dichloromethane (30 ml) and filtered through Celite. The filtrate is concentrated under reduced pressure and 1.1 g of compound are obtained in the form of a beige-coloured powder, which is used without further purification in the following step. Yield: 97%. MH+: 173.2 (tr: 0.72 min., condition 1).

1. temperatureThe reaction mixture is cooled to room temperature
2. filtrationfiltered through Celite
3. concentrationThe filtrate is concentrated under reduced pressure and 1.1 g of compound
4. customare obtained in the form of a beige-coloured powder, which
5. customis used without further purification in the following step
6. custom173.2 (tr: 0.72 min., condition 1)

ORD-Eintrag

ord-78e15b2011ae4b189ce1f236f24382e2

Quelldatensatz

uspto-grants-2013_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08436011B2