Reaktion #51605
ord-c4f7d550f4084b819d2aa770f40142bf
Reaktionsgleichung
5F
(3-Benzyloxy-5-trifluoromethylthien-2-yl)-carboxylic acid
→
liquid
Ausbeute 71.0%
3-Benzyloxy-5-trifluoromethylthiophen
Ausbeute 71.0%
Lösungsmittel
Reaktionsbedingungen
Temperatur
150°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturThe reaction mixture is heated for 25 minutes at 150° C.
- 2Temperaturcooled to room temperature
- 3FiltrationThe mixture was filtered
- 4Waschenwashed with water
- 5Extraktionextracted with diethyl ether twice
- 6WaschenThe combined organic phases were washed with water
- 7Sonstigedried
- 8EinengenThe mixture was concentrated
- 9Sonstigethe residue was chromatographed
Vorschrift
A mixture of 5F (14.5 g) and quinoline (50 ml) was treated with copper powder (4.57 g) and heated to 150° C. The reaction mixture is heated for 25 minutes at 150° C. and cooled to room temperature. The mixture was filtered and washed with water. Aqueous quinoline was acidified with 6N HCl (pH=2) and extracted with diethyl ether twice. The combined organic phases were washed with water and dried. The mixture was concentrated and the residue was chromatographed to yield a yellow liquid (8.74 g, 71%).