Triethyloxonium tetrafluoroborate → 1-[(2-Chlorophenyl)carbonyl]-3-(ethyloxy)piperazine

Temperature

25 °C

4-[(2-chlorophenyl)carbonyl]-2-piperazinone (I4) (676 mg, 2.83 mmol) was dissolved in dichloromethane (DCM) (10 mL) and was treated with triethyloxonium tetrafluoroborate (628 mg, 3.31 mmol). The solution was stirred at 25° C. for 16 hr and the solution partitioned between ethyl acetate (25 mL) and saturated sodium bicarbonate solution (25 mL). The aqueous phase was extracted with ethyl acetate (3×25 mL), combined extracts were washed with brine (25 mL), dried over anhydrous sodium sulfate and concentrated to a crude oil in 816 mg that was used in the subsequent step without further purification. Compound was not characterised but used directly in the next step.

1. customthe solution partitioned between ethyl acetate (25 mL) and saturated sodium bicarbonate solution (25 mL)
2. extractionThe aqueous phase was extracted with ethyl acetate (3×25 mL)
3. washwere washed with brine (25 mL)
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated to a crude oil in 816 mg that
6. customwas used in the subsequent step without further purification

ORD record

ord-14bb6c053b484a4e90b40085625e7b2a

Source dataset

uspto-grants-2013_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08501946B2