Reaktion #90997

ord-74e0c5cb1e9943aa826529780e22bf7a

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe mixture was partitioned between EtOAc and water
  2. 2
    Extraktionthe aqueous phase was extracted twice with EtOAc
  3. 3
    WaschenThe combined organic phases were washed with brine
  4. 4
    Trocknendried over MgSO4
  5. 5
    Filtrationfiltered
  6. 6
    Sonstigethe solvent removed in vacuo

Vorschrift

Ethanol (20 mL, 343 mmol) was treated with potassium hydroxide (956 mg, 17.0 mmol) and the mixture was stirred at RT for 1 h. A solution of 2-chloro-5-nitro-1,3-bis(trifluoromethyl)benzene (1) (1.00 g, 3.41 mmol) in DMSO (10 mL) was added dropwise. The resultant mixture was stirred at RT for 1 h. The mixture was partitioned between EtOAc and water and the aqueous phase was extracted twice with EtOAc. The combined organic phases were washed with brine, dried over MgSO4, filtered and the solvent removed in vacuo to afford 2-ethoxy-5-nitro-1,3-bis(trifluoromethyl)benzene (2) (1.00 g, 93%) as a yellow solid. 1H NMR (400 MHz, DMSO-d6) δ: 8.72 (2H, s), 4.21 (2H, q), 1.41 (3H, t).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09447028B2uspto-grants-2016_09