Hydrochloric Acid → HCID 69004781, compound

Participants

Reaction Conditions

Reaction Steps

To a cooled (0-5° C.) and stirred solution of (S)-1-[5-(3′-chloro-2-fluoro-6methoxy-biphenyl-3-ylmethyl)-pyridin-2-yl]-azetidine-2-carboxylic acid amide (P-615, 0.04 g, 0.1 mmol) in ether (2 mL) was added 2M HCl in ether (0.5 ml, 1.0 mmol), and the reaction, stirred for 1 h. The ether layer was removed, again triturated with ether (2.0 mL), concentrated to afford 0.045 g (98%) of P-615-HCl as a white solid. 1H NMR (DMSO-d6, 400 MHz): 7.92 (d, J=2.0 Hz, 1H), 7.78 (d, J=7.6 Hz, 1H), 7.69 (br s, 1H), 7.26-7.48 (m, 6H), 6.95 (d, J=8.8 Hz, 1H), 6.72 (d, J=9.2 Hz, 1H), 4.8-4.9 (m, 1H), 4.0-4.18 (m, 2H), 3.89 (s, 2H), 3.73 (s, 3H), 2.64-2.74 (m 1H), 2.26-2.34 (m, 1H) ppm; MS (APCI+): 426.16 (M+1), LC-MS: 98.8%; HPLC 98.3% pure.

Provenance & Evidence