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-6229f9a396354562be7e42eb4230bbe6

Quelldatensatz

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08841312B2