反应 #2550

ord-e6f09e6358c645c8a45e3f4af446ce3d

溶剂

反应条件

温度
80°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他equipped with a cold finger
  2. 2
    其他subsequent removal of dioxane
  3. 3
    其他by evaporation
  4. 4
    workup.ADDITIONthe resulting residue was diluted with ethyl acetate (30 ml)
  5. 5
    干燥The thus diluted solution was dried on anhydrous sodium carbonate
  6. 6
    其他the resulting residue was purified

实验过程

In an atmosphere of argon, 4-chloromethyl-N-(2-methoxyphenyl)benzamide (276 mg, 1.0 mmol) was put into a 25 ml capacity eggplant type flask equipped with a cold finger and dissolved in dioxane (3 ml), followed by the addition of 50% dimethylamine aqueous solution (3 ml) at room temperature. After 2.5 hours of stirring at 80° C. and subsequent removal of dioxane by evaporation, the resulting residue was diluted with ethyl acetate (30 ml). The thus diluted solution was dried on anhydrous sodium carbonate, and the resulting residue was purified by subjecting it to a silica gel column chromatography (ether-ethyl acetate-ethyl acetate:methanol=10:1) to obtain 284 mg (100%) of the title compound in the form of colorless oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05728835uspto-grants-1998_03