反応 #2069926

ord-8826973177f346569a29a8230f5bbb3c

反応方程式

CC(=O)N(c1ccc(C(C)C)cc1)c1ccc(C(C)C)cc1
N-Acetyl-N,N-di(4-isopropylphenyl)amine
CC(C)c1ccc(Nc2ccc(C(C)C)cc2)cc1
N,N-Di-(4-isopropylphenyl)amine

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONThe ethanolic solution is poured into dist
  2. 2
    ろ過water, and the brownish precipitate is filtered off with suction
  3. 3
    workup.DISSOLUTIONdissolved in dichloromethane
  4. 4
    乾燥dried with sodium sulphate
  5. 5
    濃縮The solution is concentrated
  6. 6
    その他chromatographed through a short silica gel column with 50% dichloromethane in hexane
  7. 7
    濃縮The product fractions are concentrated to dryness
  8. 8
    その他the product is dried under reduced pressure

実験手順

N-Acetyl-N,N-di(4-isopropylphenyl)amine (5.4 g, 18.4 mmol) are heated to reflux in 100 ml of 20% aqueous ethanol. The reaction is monitored by thin-layer chromatography. After 30 h, no reactant is any longer detectable in the TLC. The ethanolic solution is poured into dist. water, and the brownish precipitate is filtered off with suction, dissolved in dichloromethane and dried with sodium sulphate. The solution is concentrated and chromatographed through a short silica gel column with 50% dichloromethane in hexane. The product fractions are concentrated to dryness and the product is dried under reduced pressure.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07540978B2uspto-grants-2009_06