Reaktion #1127580

ord-9048f96c758b4c56967335ca56e32ee4

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    WaschenThe solution was washed with 1N HCl, saturated NaHCO3 aqueous solution, brine
  2. 2
    Trocknendried over MgSO4
  3. 3
    FiltrationAfter filtration
  4. 4
    Einengenthe filtrate was concentrated in vacuo

Vorschrift

To a solution of 2-formylbenzoic acid (500 mg, 3.33 mmol), N,N-diisopropylethylamine (0.58 mL, 3.3 mmol), and dimethylamine/ethanol solution (1.2 mL, 5.6 M, 6.7 mmol) in 3.3 mL of dichloromethane was added 1-ethyl-3-(3-dimethylaminopropyl)-3-ethylcarbodiimide monohydrochloride (1.28 g, 6.67 mmol) at 0° C. After being stirred at room temperature overnight, the reaction mixture was diluted with diethyl ether. The solution was washed with 1N HCl, saturated NaHCO3 aqueous solution, brine, and dried over MgSO4. After filtration, the filtrate was concentrated in vacuo to obtain the title compound as a slightly yellow oil (113 mg, 19%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08552220B2uspto-grants-2013_10