Water → HCID 20376744, Verbindung

Temperatur

100 °C

To a mixture of 4,5-dichloro-2-nitro-phenylamine (1.29 g, 6.23 mmol) and dry MeOH (2 mL), a 25 wt % solution of sodium methoxide in MeOH (10 mL) was added and the mixture stirred for 6 h at 100° C. in a sealed tube. The mixture was cooled to 23° C., poured into water (50 mL), and extracted with EtOAc (3×50 mL). The combined organic layers were washed with brine (25 mL), dried, filtered, and concentrated under reduced pressure to afford the titled compound (0.700 g, 56%). The crude material was used without further purification in the next reaction.

1. temperatureThe mixture was cooled to 23° C.
2. extractionextracted with EtOAc (3×50 mL)
3. washThe combined organic layers were washed with brine (25 mL)
4. customdried
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure

ORD-Eintrag

ord-672c580f1ebb4242874e1b64d5ae7e04

Quelldatensatz

uspto-grants-2014_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08759345B2