反应 #2069926

ord-8826973177f346569a29a8230f5bbb3c

反应方程式

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

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

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