反応 #1135812

ord-45624fadc49d46e9aa387dbc6f610bda

反応方程式

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
収率 100.7%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度with heating
  2. 2
    温度under reflux for ten hours
  3. 3
    ろ過filtered
  4. 4
    濃縮the resulting filtrates were concentrated
  5. 5
    抽出The resulting mixtures were extracted with ethyl acetate
  6. 6
    洗浄the organic layers were washed with water and saturated saline
  7. 7
    乾燥were dried over anhydrous magnesium sulfate
  8. 8
    濃縮were then concentrated under reduced pressure

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09380782B2uspto-grants-2016_07