Hydrochloric Acid → HCID 10304683, compound

Participants

Reaction Steps

To a 150 mL round-bottomed flask equipped with stirring was added tert-butyl(3S)-3-(N-[(1R)-1-[(3,4-dichlorophenyl)methyl]-2-(4-{2-[(methylsulfonyl)-amino]phenyl)piperidyl)-2-oxoethyl]carbamoyl}-1,2,3,4-tetrahydroisoquinoline-2-carboxylate (Step b) (0.54 g, 0.74 mmol) followed by a saturated soln of HCl in EtOAc (50 mL). The reaction mixture was stirred at RT for 1 h and concentrated in vacuo to a white solid. Recrystallization from MeOH:Et2O (1:20) provided the title compound (HCl salt) as a white solid (0.3 g). MP 181° C. (decomposed). MS (ESI, pos. ion) m/z: 629 (M+1); MS (ESI, neg. ion) m/z: 627 (M−1). Calc'd for C31H34Cl2N4O4S: 628.17. Anal. Calcd for C31H34Cl2N4O4S.HC].H2O: C, 51.71; H, 5.74; N, 7.78; Cl, 14.77. Found: C, 51.66; H, 5.39; N, 7.49; Cl, 15.07.

Provenance & Evidence