Dimethylformamide → HCID 58817541, compound

Temperature

60 °C

To a room temperature solution of (1-benzyl-piperidin-4-yl)-(2-fluoro-4-trifluoromethyl-phenyl)-methanone (7.5 g, 20.5 mmol), methyl thioglycolate (2.0 mL, 22.5 mmol), and DMF (100 mL) was added K2CO3 (5.65 g, 41.0 mmol). The reaction was stirred at 60° C. for 24 hours, cooled to room temperature and diluted with ethyl acetate (500 mL). The mixture was washed with water (2×300 mL) and brine (300 mL) successively, dried over magnesium sulfate, filtered, and the solvent removed to afford an oil. The oil was purified via chromatography (30% EtOAc in heptane) yielding 5.91 g (67%) as a solid.

1. temperaturecooled to room temperature
2. washThe mixture was washed with water (2×300 mL) and brine (300 mL) successively
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. customthe solvent removed
6. customto afford an oil
7. customThe oil was purified via chromatography (30% EtOAc in heptane)
8. customyielding 5.91 g (67%) as a solid

ORD record

ord-a811474e00cf48cb84622304de518e59

Source dataset

uspto-grants-2010_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07772252B2