Reaktion #480093

ord-7b785364b4ab40d099bc0268f05733f4

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled
  2. 2
    Waschenwashed with water (3×25 mL), brine (1×25 mL)
  3. 3
    Trocknendried (Na2SO4)
  4. 4
    Filtrationfiltered
  5. 5
    Einengenconcentrated

Vorschrift

Cesium carbonate (2.24 g, 6.9 mmol) was added to a solution of 2-hydroxy-5-trifluoromethyl-benzyl alcohol (885 mg, 4.6 mmol) and benzyl bromide (547 μL, 4.6 mmol) in anhydrous DMF (8 mL) at room temperature. The reaction was heated to 50° C. for 2 hours, cooled, diluted with ethyl acetate (25 mL) and washed with water (3×25 mL), brine (1×25 mL), and dried (Na2SO4), filtered and concentrated to afford 1.3 g of the title compound as a colorless solid. 1H NMR (400 MHz. CDCl3) δ 7.6-7.3 (m, 7H); 7.01 (d, 1H, J=9.1 Hz); 5.18 (s, 2H); 4.79 (s, 2H); 2.8 (bs, 1H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06803457B1uspto-grants-2004_10