p-Fluorophenethylamine → HCID 7935360, Verbindung

A 250-mL, round-bottomed flask containing a solution of 4-fluorophenethylamine (4.8 mL, 37 mmol) and diisopropylethylamine (6.4 mL, 37 mmol) in dichloromethane (40 mL) was cooled to 0° C. and treated dropwise with 4-(trifluoromethyl)benzoyl chloride (5.5 mL, 37 mmol) over 5 min. The ice-bath was removed after 2 h and the reaction mixture was stirred overnight. The precipitate formed was collected by filtration. The filtrate was diluted with dichloromethane (100 mL) and transferred to a separatory funnel, extracted with water (35 mL), brine (25 mL), and 1N HCl (25 mL). The dichloromethane layer was separated and formation of more precipitate was observed which was collected by filtration. The solids collected were combined and dried under vacuum to yield N-(4-fluorophenethyl)-4-(trifluoromethyl)benzamide as an off-white solid. MS (ESI pos. ion) m/z: 312 (M+H).

1. customThe ice-bath was removed after 2 h
2. customThe precipitate formed
3. filtrationwas collected by filtration
4. additionThe filtrate was diluted with dichloromethane (100 mL)
5. customtransferred to a separatory funnel
6. extractionextracted with water (35 mL), brine (25 mL), and 1N HCl (25 mL)
7. customThe dichloromethane layer was separated
8. filtrationwas collected by filtration
9. customThe solids collected
10. customdried under vacuum

ORD-Eintrag

ord-130f064c968347e7b6b87e75f5c8b373

Quelldatensatz

uspto-grants-2013_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08476297B2