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 기록

ord-05527076ac39450292df252249039a8a

출처 데이터셋

uspto-grants-2010_07

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07749992B2