Pyridine → N-(1-Acetyl-8-chloro-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yl)-N-(3,5-bis-trifluoromethyl-benzyl)-acetamide

Add acetyl chloride (0.3 mmol) followed by dimethylaminopyridine (cat.) and pyridine (0.3 mmol) to a solution of N-(3,5-Bis-trifluoromethyl-benzyl)-N-(8-chloro-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yl)-acetamide (0.05 g, 0.11 mmol) in dichloromethane (1 ml). After stirring for 14-16 h dilute with dichloromethane (2 mL) and wash with 5% HCl (2 mL), water (2 mL) and brine (2 mL). Dry the organics over sodium sulfate, filter, and remove solvent under vacuum. Chromatograph the crude product over silica gel using ethyl acetate/hexane (10-30%) to elute. This afford the title compound (0.04 g, 89%) as a colorless solid: MS (ES+): 507 (M+H).

1. washwash with 5% HCl (2 mL), water (2 mL) and brine (2 mL)
2. dry with materialDry the organics over sodium sulfate
3. filtrationfilter
4. customremove solvent under vacuum
5. washto elute

ORD-Eintrag

ord-05527076ac39450292df252249039a8a

Quelldatensatz

uspto-grants-2010_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07749992B2