Reaktion #335165

ord-d09ecf70b30b4f1d882d81c75e4cfcf2

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturby heating
  2. 2
    Temperaturat reflux temperature for 6 hours
  3. 3
    SonstigeThe residue is purified by column chromatography (silica gel: 80% ethyl acetate/hexane)

Vorschrift

The title compound is prepared by the procedure of Example 27 using 2.45 g of product from Example 22, 0.960 g of product from Example 12, 0.322 g of washed 50% sodium hydride and 30 ml of tetrahydrofuran. The reaction is stirred at 0° C. for 1 hour, room temperature for 18 hours; followed by heating at reflux temperature for 6 hours. The residue is purified by column chromatography (silica gel: 80% ethyl acetate/hexane) to give 0.976 g of the desired product as a yellow oil. The spectral data shows the presence of 2 rotomers.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05208247uspto-grants-1993_05