Reaktion #463453

ord-6ed914aae22f4d22951d8ded0091096c

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reaction mixture was quenched with 2N sulphuric acid (250 ml)
  2. 2
    Extraktionextracted with ether (3×250 ml))
  3. 3
    TrocknenThe combined organics were dried (Na2SO4)
  4. 4
    Sonstigeevaporated
  5. 5
    Sonstigeto give a dark yellow oil
  6. 6
    SonstigePurification by FCC (hexane/ether (2:1))

Vorschrift

A solution of 4-(5-trifluoromethyl-tetrazol-1-yl)-phenol (45 mmol) in trifluoroacetic acid (200 ml) and hexamethylenetetramine (186.9 mmol) was heated at 100° under nitrogen for 16 h. The reaction mixture was quenched with 2N sulphuric acid (250 ml) and extracted with ether (3×250 ml)). The combined organics were dried (Na2SO4) and evaporated to give a dark yellow oil. Purification by FCC (hexane/ether (2:1)) afforded the title compound (8.8 g) as a pale yellow solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06020346uspto-grants-2000_02