Ammonia → 5-Bromo-N4-(tetrahydro-pyran-4-yl)-pyrimidine-2,4-diamine

Temperatur

130 °C

To a suspension of compound 32 (6.60 g, 23 mmol) in isopropyl alcohol (40 ml) was added ammonia (aq. 28%, 80 ml). This reaction mixture was heated to 130° C. for 14 hours in a pressure vessel. The reaction mixture was cooled down to room temperature and to this mixture was added ethyl acetate. The reaction mixture was washed with water and brine. The ethyl acetate layer was dried with sodium sulfate and concentrated to give compound 33 (4.75 g, 77%). 1H NMR (500 MHz, CD3OD) δ ppm 7.79 (1 H, s), 4.24 (1 H, m), 3.99-4.02 (2 H, dd, J=11.0, 2.2 Hz), 3.52 (2 H, td, J=11.9, 2.0 Hz), 1.92-1.96 (2 H, m), 1.69 (2 H, m); LCMS-ESI (POS), M/Z, M+1: Found 273, Calculated 273.0

1. temperatureThe reaction mixture was cooled down to room temperature and to this mixture
2. washThe reaction mixture was washed with water and brine
3. dry with materialThe ethyl acetate layer was dried with sodium sulfate
4. concentrationconcentrated

ORD-Eintrag

ord-4ed4a0daf9b74ca28c30c9bd6c07c2a6

Quelldatensatz

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08980903B2