Reaktion #2178363

ord-254d791e4a0e4343b2a0e2999078246e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwith heating
  2. 2
    Temperaturunder reflux
  3. 3
    Einengenconcentrated under reduced pressure
  4. 4
    workup.DISSOLUTIONThe residue was dissolved in water (10 mL)
  5. 5
    workup.ADDITION1N hydrochloric acid (5.00 mL) was added at 0° C
  6. 6
    FiltrationThe resulting precipitate was collected by filtration

Vorschrift

To a mixture of methyl 4-{[2-ethyl-1-(5-methoxy-3-methyl-1-benzofuran-2-yl)butyl]amino}benzoate (718 mg) synthesized above, tetrahydrofuran (5 mL) and ethanol (5 mL) was added 1N aqueous sodium hydroxide solution (5.00 mL), and the mixture was stirred overnight with heating under reflux, and concentrated under reduced pressure. The residue was dissolved in water (10 mL), and 1N hydrochloric acid (5.00 mL) was added at 0° C. The resulting precipitate was collected by filtration to give the title object compound (574 mg, 83%) as a white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08436043B2uspto-grants-2013_05