Hydrochloric Acid → HCID 45072358, compound

To a round bottom flask containing (R)—N—((S)-1-(2,3-difluorophenyl)ethyl)-2-methylpropane-2-sulfinamide (786.8 mg, 3.01 mmol) was added Dioxane (10.000 mL). To this solution was added HCl in dioxane 4.0M (1.505 mL, 6.02 mmol) and the solution was allowed to stir 15 min at room temperature. The reaction mixture was concentrated, dissolved in Et2O 10 ml, and concentrated again. Et2O was again added and resulting mixture sonnicated and a solid material was filtered and dried to afford (S)-1-(2,3-difluorophenyl)ethanamine (0.4213 g, 2.176 mmol, 72.3% yield) as a white crystalline HCl salt. 1H NMR (400 MHz, D20) d ppm 1.55 (d, J=6.99 Hz, 3H) 4.71 (q, J=6.96 Hz, 1H) 7.10-7.26 (m, 3H); LCMS m/z 158.0 (M+H)+, Rt 0.37 min.

1. concentrationThe reaction mixture was concentrated
2. dissolutiondissolved in Et2O 10 ml
3. concentrationconcentrated again
4. additionEt2O was again added
5. customresulting mixture
6. filtrationa solid material was filtered
7. customdried

ORD record

ord-9d81a519c7ce478f9995a2bd1c5c6bd6

Source dataset

uspto-grants-2015_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08957068B2