Reaktion #344915

ord-e499b1e1b3ff402c89419ebaf7537efe

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethen quenched
  2. 2
    workup.ADDITIONby adding 20 mL of water and 75 mL of ether
  3. 3
    WaschenThe ether was washed with 50 mL water
  4. 4
    Extraktionthe aqueous phase was extracted with 50 ml ethyl acetate
  5. 5
    TrocknenThe ether was dried
  6. 6
    Einengenconcentrated

Vorschrift

To a 100 mL 3 neck flask stirring under nitrogen was charged 1.5 g (0.9375 mole) 60% sodium hydride (prewashed with hexanes) in 50 mL of dimethyl formamide. To the slurry was charged 3.83 g (0.0125 mole) of 2-(4-chlorophenyl)-2-[(1,2,4-triazol-1-yl)methyl]hexanamide in 50 mL of dimethyl formamide. The mixture was stirred at room temperature for 3 hours then quenched by adding 20 mL of water and 75 mL of ether. The ether was washed with 50 mL water and the aqueous phase was extracted with 50 ml ethyl acetate. The ether was dried and concentrated and gave 1.88 g (45.1% yield) of product as an oil, Example 160 of Table 1.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05264415uspto-grants-1993_11