Reaktion #1915078

ord-f193044562254a25978d71b924c37984

Reaktionsbedingungen

Temperatur
160°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe vial was sealed
  2. 2
    Sonstigeabsorption level normal
  3. 3
    TemperaturIt was then cooled to room temperature
  4. 4
    workup.ADDITIONdiluted with 2 mL of methanol
  5. 5
    Sonstigepurified by semi-prep HPLC
  6. 6
    SonstigeThe HPLC fractions were evaporated under reduced pressure

Vorschrift

2-amino-4-phenylphenol (0.180 g, 0.97 mmol) was placed in a Smith Process Vial™ (Personal Chemistry, Inc., Uppsala) (3 mL glass vessel) followed by the addition of 1-chloro-2,2,2-trimethoxyethane (1 mL). The vial was sealed and the mixture was heated in the Emrys Optimizer™ (Personal Chemistry, Inc., Uppsala) microwave at 160° C. for 300 s, fixed hold time on, absorption level normal, pre-stirring 10 s. It was then cooled to room temperature, diluted with 2 mL of methanol and purified by semi-prep HPLC. The HPLC fractions were evaporated under reduced pressure to furnish 2-(chloromethyl)-5-phenyl-benzoxazole as an off-white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07056924B2uspto-grants-2006_06