Reaktion #361158

ord-a6adfda3bf624cce8cb2ec246b607b90

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationAfter filtering off the salts
  2. 2
    Einengenthe reaction mixture is concentrated in vacuo
  3. 3
    Sonstigeleaving a golden oil

Vorschrift

A mixture of 4.12 g of α-chloro-3,4-dimethoxybenzeneacetonitrile (U.S. Pat. No. 4,833,162), 2.48 g of p-thiocresol, 2.76 g of potassium carbonate and 100 mL of acetonitrile is stirred at 65° C. overnight. After filtering off the salts, the reaction mixture is concentrated in vacuo leaving a golden oil. The oil is dissolved in a minimum amount of ethyl acetate and diluted with 3 volumes of hexane. Seeding gives 3.81 g of the desired compound as light yellow crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05387685uspto-grants-1995_02