Isobutyryl chloride → HCID 18538606, Verbindung

To a stirred solution of 4-benzyl-1-(trifluoroacetyl)piperidine (4.34 g, 16.0 mmol) and isobutyryl chloride (2.18 mL, 20.8 mmol) in dichloromethane (50 mL) was added aluminum chloride (5.33 g, 40.0 mmol) at 0° C., and the reaction mixture was stirred at room temperature for 3 hours. The reaction mixture was poured into ice water (50 g), the organic layer was separated and the aqueous layer was extracted with dichloromethane (30 mL) The combined organic layers were washed with saturated aqueous sodium bicarbonate solution (3×15 mL), brine (15 mL), dried over anhydrous magnesium sulfate, filtered, and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel, using ethyl acetate/hexane (1/19 to 1/9) as eluent to afford the title compound (3.60 g, 10.5 mmol, 66%) as a colorless oil.

1. customthe organic layer was separated
2. extractionthe aqueous layer was extracted with dichloromethane (30 mL) The combined organic layers
3. washwere washed with saturated aqueous sodium bicarbonate solution (3×15 mL), brine (15 mL)
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationfiltered
6. customevaporated under reduced pressure
7. customThe residue was purified by column chromatography on silica gel

ORD-Eintrag

ord-c5a73df50a604f5bb5c36537d62d3768

Quelldatensatz

uspto-grants-2003_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06562978B1