2-Amino-1-[4-(methylsulfonyl)phenyl]-1-ethanone hydrochloride synthesis

Yield:102871-96-5 53%

Reaction Conditions:

with hydrogenchloride in ethanol;water at 50; for 2 h;

Steps:

215.3 2-Amino-1-(4-(methylsulfonyl)phenyl)ethanone hydrochloride

To the solution of concentrated HCI (10 mL) in EtOH (40 mL) was added 2- amino-1-(4-(methylsulfonyl)phenyl)ethanone (7.2 g, 17.3 mmol) at RT. Themixture was stirred for 2 h at 50 C After cooling to 5 C the resulting white solid was collected by filtration, washed with EtOH (10 mL). The solid was dissolved in the mixture of H20 (12 mL) and concentrated HCI (0.5 mL) at 70 C the hot solution was filtered and the filtrate was cooled to 5 C the crystalline white solid was isolated by filtration, washed with ice-cold H20 (5 mL) and EtOH (5 mL),dried under high vacuum to afford the product (2.30 g, 9.2 mmol, 53 %). 1H NMR (400 MHz, D20): O = 3.17 (d, J= 2.8 Hz, 2 H), 4.64 (s, 3 H), 7.99 (m, 2 H), 8.09(m, 2 H) ppm.

References:

WO2015/187088,2015,A1 Location in patent:Page/Page column 126; 127