Potassium Carbonate → tert-Butyl (2-((5-methoxy-2-nitrophenyl)amino)ethyl)carbamate

HRID 1914920

Reaktionsgleichung

C([O-])([O-])=O.[K+].[K+].[CH3:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[C:11](F)[CH:10]=1.[C:19]([NH:26][CH2:27][CH2:28][NH2:29])([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20]>CS(C)=O>[C:22]([O:21][C:19](=[O:20])[NH:26][CH2:27][CH2:28][NH:29][C:11]1[CH:10]=[C:9]([O:8][CH3:7])[CH:14]=[CH:13][C:12]=1[N+:15]([O-:17])=[O:16])([CH3:25])([CH3:23])[CH3:24]

Komponenten

Reaktionsbedingungen

Temperatur: 60 °C

Versuchsvorschrift

A 2 L flask equipped with a stir bar was charged with DMSO (800 mL), K2CO3 (161 g, 1.6 mol) and 4-methoxy-2-fluoro-1-nitrobenzene (100 g, 0.58 mol). Mono-N-Boc-1,2-diaminoethane (94 g, 0.55 mol) was added to the reaction mixture and stirred for 12 h at 60° C. The reaction mixture was triturated with ice cold water (1.2 L) and the resulting yellow precipitate was collected by vacuum filtration. The precipitate was washed several times with water (5×1 L) and dried on a high vacuum for 48 h to give the desired product as a bright yellow solid (178 g, 98%.)

Aufarbeitung

customA 2 L flask equipped with a stir bar
customThe reaction mixture was triturated with ice cold water (1.2 L)
filtrationthe resulting yellow precipitate was collected by vacuum filtration
washThe precipitate was washed several times with water (5×1 L)
customdried on a high vacuum for 48 h

Quellen und Nachweise

ORD-Eintrag: ord-c416f85f63e34c768e0fc40e299a8a2e
Quelldatensatz: uspto-grants-2013_12
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08614243B2

Verknüpfte Notizen

Wird geladen…