Reaktion #1135812

ord-45624fadc49d46e9aa387dbc6f610bda

Reaktionsgleichung

Cc1c(O)cccc1[N+](=O)[O-]
2-methyl-3-nitrophenol
CCI
iodoethane
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CCOc1cccc([N+](=O)[O-])c1C
1-ethoxy-2-methyl-3-nitrobenzene
Ausbeute 100.7%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwith heating
  2. 2
    Temperaturunder reflux for ten hours
  3. 3
    Filtrationfiltered
  4. 4
    Einengenthe resulting filtrates were concentrated
  5. 5
    ExtraktionThe resulting mixtures were extracted with ethyl acetate
  6. 6
    Waschenthe organic layers were washed with water and saturated saline
  7. 7
    Trocknenwere dried over anhydrous magnesium sulfate
  8. 8
    Einengenwere then concentrated under reduced pressure

Vorschrift

A mixture of 2-methyl-3-nitrophenol 33.5 g, iodoethane 41 g and potassium carbonate 90 g in acetone 400 mL was stirred with heating under reflux for ten hours. The mixtures were cooled to room temperature and filtered and the resulting filtrates were concentrated. The resulting mixtures were extracted with ethyl acetate and the organic layers were washed with water and saturated saline, and were dried over anhydrous magnesium sulfate and were then concentrated under reduced pressure. The resulting residues were subjected to a silica gel column chromatography to give 1-ethoxy-2-methyl-3-nitrobenzene 39.9 g.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09380782B2uspto-grants-2016_07