Reaktion #330800

ord-b472de72cd7748458a13dbf5c0288e17

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reaction was quenched
  2. 2
    workup.ADDITIONby pouring it into 100 g of ice
  3. 3
    ExtraktionThe reaction was extracted with chloroform (3×)
  4. 4
    Waschenwashed with cold water (2×)
  5. 5
    Trocknendried over MgSO4
  6. 6
    Filtrationfiltered
  7. 7
    Einengenconcentrated

Vorschrift

To a solution of chlorosulfonic acid (12.0 mL, 180 mmol) at 0° C. was added 2-nitrophenol (8.35 g, 60.0 mmol) in small portions over 1 h. The reaction was heated to 60° C. for 20 minutes and allowed to stir for 18 h at 25 C. The reaction was quenched by pouring it into 100 g of ice. The reaction was extracted with chloroform (3×), washed with cold water (2×), dried over MgSO4, filtered, and concentrated to give 9.06 g (64%) of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08653141B2uspto-grants-2014_02