4-Methylmorpholine → HCID 66791762、化合物

関与物質

反応手順

(R)-4-chloro-1-(3-methoxypropyl)-2-(piperidin-3-yl)-1H-benzo[d]imidazole (0.245 mmol, crude oil) (48A) was added to a 15 mL round-bottomed flask equipped for stirring under nitrogen. DMF (2 mL), (R)-4-(4-bromophenyl)-3-(tert-butoxycarbonylamino)butanoic acid (0.319 mmol, 0.082 g) and N-methylmorpholine (1.47 mmol, 0.162 mL) were then added and the solution was allowed to stir at rt for 5 min. HATU (0.319 mmol, 0.121 g) was added and the resultant solution was stirred at room temperature for 3 hr. The reaction solution was then directly purified by preparative LC/MS (25-85% CH3CN in H2O). The resultant fractions were collected and the solvent was removed in-vacuo affording tert-Butyl (R)-1-(4-bromophenyl)-4-((R)-3-(4-chloro-1-(3-methoxypropyl)-1H-benzo[d]imidazol-2-yl)piperidin-1-yl)-4-oxobutan-2-ylcarbamate (48B) as a clear oil which was used without further quantification. ESI-ESI-MS: m/z 647.3 (M+H)+.

情報源と証拠