Hydrochloric Acid → HCID 22464461, compound

Temperature

65 °C

To a stirred solution of 2-(ethylsulfonyl)benzyltrifluoroacetamide (88 mg, 0.30 mmol) in methanol (11 mL) and water (0.74 mL) was added potassium carbonate (124 mg, 0.90 mmol). The mixture was heated to 65° C. and stirred under Ar overnight. The mixture was then concentrated to a colorless oil which was taken up in EtOAc and washed with a small amount of brine. The aqueous layer was extracted twice with CHCl3 and was then saturated with sodium chloride and further extracted with THF. The combined organic extracts were dried over MgSO4 and concentrated at reduced pressure. The residue was treated with 2 equivalents of 1.0 M HCl in ether. The resulting precipitate was collected by filtration and was dried on a high vacuum line to give the title compound as an off-white solid:

1. concentrationThe mixture was then concentrated to a colorless oil which
2. washwashed with a small amount of brine
3. extractionThe aqueous layer was extracted twice with CHCl3
4. extractionsaturated with sodium chloride and further extracted with THF
5. dry with materialThe combined organic extracts were dried over MgSO4
6. concentrationconcentrated at reduced pressure
7. filtrationThe resulting precipitate was collected by filtration
8. customwas dried on a high vacuum line

ORD record

ord-19b912a4905f4e86911fde79cb494313

Source dataset

uspto-grants-2002_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06387911B1