Reaktion #77981
ord-d308b8da7bb94c82a8950bd040312d69
Reaktionsgleichung
Reagenzien
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturwas heated
- 2Temperaturat reflux temperature for 3 hours
- 3Sonstigethen evaporated
- 4workup.DISSOLUTIONThe residue was dissolved in tert-butyl methylether
- 5Waschenthe solution was washed with saturated aqueous sodium bicarbonate solution
- 6Trocknenwith water, then dried
- 7Sonstigeevaporated
Vorschrift
A solution of 3-hydroxy-4-nitrophenylacetic acid (4.0 g, prepared according to the procedure described by Meyer et al, J.Med.Chem., 1997, 40, pages 1049-1062) in ethanol (approximately 100 mL) was treated with concentrated hydrochloric acid (5-8 drops) was heated at reflux temperature for 3 hours then evaporated. The residue was dissolved in tert-butyl methylether and the solution was washed with saturated aqueous sodium bicarbonate solution, then with water, then dried, and then evaporated to give the title compound (5.0 g) as a light yellow solid.