Trichloroacetyl chloride → HCID 70922409, compound

Temperature

45 °C

To a solution of 2,2,2-trichloroacetyl chloride (5.05 mL, 45.3 mmol) in dry diethyl ether (12 mL) was slowly added a solution of 3-methyl-1H-pyrrole (3.15 g, 39.37 mmol) in 30 mL of dry diethyl ether during 1 h 15 min. Once the addition was finished, the reaction mixture was stirred at 45° C. during 1 hour 30 minutes more. Next, more diethyl ether was added and the organic phase was washed with an aqueous solution of potassium carbonate to neutralize de media, water and brine. The organic phase was dried (Na2SO4) and concentrated to dryness to give a residue that was purified by flash chromatography silica (hexane/dichloromethane) to afford 4.7 g of the title compound (55% yield).

1. additionOnce the addition
2. washthe organic phase was washed with an aqueous solution of potassium carbonate
3. dry with materialThe organic phase was dried (Na2SO4)
4. concentrationconcentrated to dryness
5. customto give a residue that
6. customwas purified by flash chromatography silica (hexane/dichloromethane)

ORD record

ord-d8226630e89d4b779ad86ddefaff351f

Source dataset

uspto-grants-2016_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09340547B2