Reaktion #2151302

Reaktionsgleichung

diisopropylethylamine

1,1-dimethylethyl 4-amino-1-piperidinecarboxylate

1-Chloro-2,5-difluoro-4-nitrobenzene

water

→

title compound

1,1-Dimethylethyl 4-[(5-chloro-4-fluoro-2-nitrophenyl)amino]-piperidinecarboxylate

Lösungsmittel

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe aqueous solution was extracted with ethyl acetate (2×)
2. 2
   Waschenorganics were alternatively washed with brine and water (2×)
3. 3
   TrocknenThe organics were combined dried over Na2SO4
4. 4
   Filtrationfiltered
5. 5
   Sonstigethe solvent was evaporated

Vorschrift

1-Chloro-2,5-difluoro-4-nitrobenzene (D1) (1.18 mmol, 228 mg) was dissolved in dry dimethylformamide (2 ml) and diisopropylethylamine (1 eq., 1.18 mmol, 0.209 ml), 1,1-dimethylethyl 4-amino-1-piperidinecarboxylate (1 eq., 1.18 mmol, 236 mg) were added at room temperature and the mixture was stirred at 50° C. overnight. The crude mixture was then cooled to room temperature and water (150 ml) was added; the aqueous solution was extracted with ethyl acetate (2×); organics were alternatively washed with brine and water (2×). The organics were combined dried over Na2SO4, filtered and the solvent was evaporated to afford the title compound, 340 mg, 80%, bright orange solid, M+−H=372.

Quelle