Water → 3,5-Dichloro-4-(2-(dimethylamino)acetamido)-benzylamine

Temperatur

0 °C

Step F (3): To a solution of the compound of step F (2) (6 g 0.014 mol) in dry DMF (60 ml) under N2, anhydrous K2CO3 (6.03 g, 0.043 mol) was added with stirring. The reaction mixture was cooled to 0° C. and N,N-dimethylamine hydrochloride (2.37 g, 0.029 mol) was added at once. The reaction mixture was allowed stir for overnight at room temperature. The reaction mixture was poured into water and extracted with ethyl acetate (2×150 ml). The organic layer was washed with water (25 ml), brine (25 ml), dried over anhydrous sodium sulfate and concentrated under vacuum to remove the volatiles. The resulting crude product was purified by column chromatography using CHCl3: MeOH (9:1) as eluent to afford the product as an off-white solid (4 g, 72.9%)

1. stirringThe reaction mixture was allowed stir for overnight at room temperature
2. extractionextracted with ethyl acetate (2×150 ml)
3. washThe organic layer was washed with water (25 ml), brine (25 ml)
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated under vacuum
6. customto remove the volatiles
7. customThe resulting crude product was purified by column chromatography

ORD-Eintrag

ord-41fa60e5165f4223ab538e5e900bb772

Quelldatensatz

uspto-grants-2008_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07390925B2