Reaktion #77981

ord-d308b8da7bb94c82a8950bd040312d69

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturat reflux temperature for 3 hours
  3. 3
    Sonstigethen evaporated
  4. 4
    workup.DISSOLUTIONThe residue was dissolved in tert-butyl methylether
  5. 5
    Waschenthe solution was washed with saturated aqueous sodium bicarbonate solution
  6. 6
    Trocknenwith water, then dried
  7. 7
    Sonstigeevaporated

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06706738B2uspto-grants-2004_03