Hydrochloric Acid → Ethyl 2-(4-bromo-2-nitrophenyl)acetate

To a stirred solution of concentrated HCl (18.00 mL) diluted to 72.00 mL with 95% Ethanol was added 2-(4-bromo-2-nitro-phenyl)-malonic acid diethyl ester (2.50 g, 6.94 mmol). The resulting mixture was then heated at reflux under N2 for 4 h. The reaction mixture was allowed to cool to ambient temperature and poured into H2O (250 mL). This aqueous mixture was then extracted with 2×150 mL of Diethyl ether. The Et2O layer was extracted with H2O and 5% NaHCO3 washed with brine, dried (MgSO4), and filtered. Evaporation of the filtrate in vacuo gave the intermediate title compound as a yellow liquid (1.52 g, 76%).

1. temperatureThe resulting mixture was then heated
2. temperatureat reflux under N2 for 4 h
3. extractionThis aqueous mixture was then extracted with 2×150 mL of Diethyl ether
4. extractionThe Et2O layer was extracted with H2O and 5% NaHCO3
5. washwashed with brine
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. customEvaporation of the filtrate in vacuo

ORD-Eintrag

ord-041985fb1d65411aac1280d05aeb1246

Quelldatensatz

uspto-grants-2006_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07034045B1