Réaction #70920

ord-badfea930b6a45b793feba79f82ae152

Conditions de réaction

Température
80°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températurecooled to room temperature
  2. 2
    FiltrationThe precipitate was filtered off
  3. 3
    Lavagewashed with water
  4. 4
    Autredried

Mode opératoire

To a stirred solution of 3-methoxy-5-nitro-3′-(6-(trifluoromethyl)pyridin-2-yl)biphenyl-4-ol (0.288 g, 0.738 mmol) in 1,2-dichloroethane (10 mL) cooled in an ice-water bath was added aluminium chloride (0.123 g, 0.922 mmol) in one portion followed by pyridine 0.233 g, 2.95 mmol) dropwise. The resulting red suspension was stirred at 80° C. for two hours, then cooled to room temperature and poured onto cold 2 N aqueous hydrochloric acid (100 mL). The precipitate was filtered off, washed with water and dried to give 5-nitro-3′-(6-(trifluoromethyl)pyridin-2-yl)biphenyl-3,4-diol, 0.164 g, (59%).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08536203B2uspto-grants-2013_09