Reaktion #1072036

Reaktionsgleichung

1-(2-fluoro-3-methoxy-6-nitrophenyl)-propan-2-one

pyridinium chloride

→

1-(2-fluoro-3-hydroxy-6-nitrophenyl)-propan-2-one

Ausbeute 96.0%

Lösungsmittel

HCl

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction was cooled to room temperature
2. 2
   Filtrationfiltered
3. 3
   WaschenThe filtrate was washed with brine (2×)
4. 4
   Sonstigedried
5. 5
   Einengenconcentrated in vacuo

Vorschrift

A mixture of 1-(2-fluoro-3-methoxy-6-nitrophenyl)-propan-2-one from previous step (454 mg, 21 mmol) and pyridinium chloride (0.9 g, 7.8 mmol) was stirred at 180° C. for 75 min. The reaction was cooled to room temperature, diluted with 1N HCl (3 mL) and ethyl acetate (10 mL) and filtered. The filtrate was washed with brine (2×), dried and concentrated in vacuo to give 1-(2-fluoro-3-hydroxy-6-nitrophenyl)-propan-2-one (410 mg, 96%) as a grey solid, which was used without further purification for the next step. LC/MS; (M+H)+=214. 1HNMR (CDCl3): δ 2.37 (s, 3H), 4.22 (s, 2H), 6.95 (dd, 1H), 7.95 (d, 1H, J=9.35 Hz).

Quelle