Methylamine → [(1R)-1-(4-bromophenyl)-2-(4-morpholinyl)ethyl]methylamine

Temperatur

0 °C

Crude 4-[(2R)-2-(4-Bromophenyl)-2-chloroethyl]morpholine (34.5 g) was dissolved in 200 mL of EtOH at room temperature with magnetic stirring. The resulting solution was cooled to 0° C. and treated with 71 ml of MeNH2 (33 wt % in EtOH) under N2. The reaction flask was capped by a rubber septum, and the reaction mixture was maintained at room temperature for 48 h. The reaction mixture was concentrated, and the residue was partitioned between EtOAc and sat NaHCO3(aq). The organic layer was washed by brine, dried over MgSO4, and filtered. The filtrate was concentrated to yield the title compound as a yellow solid (31.6 g, 93%). MS (ES) m/e 300, 301 [M+H]+.

1. customThe reaction flask was capped by a rubber septum
2. temperaturethe reaction mixture was maintained at room temperature for 48 h
3. concentrationThe reaction mixture was concentrated
4. customthe residue was partitioned between EtOAc
5. washThe organic layer was washed by brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationThe filtrate was concentrated

ORD-Eintrag

ord-a23b0d34467d4897a980a9678a6e0713

Quelldatensatz

uspto-grants-2010_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07749998B2