HRID345046

反应详情

EQUATION

反应方程式

HRID 345046 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of the product of part (A) above (3.20 g), N-methyl-4-nitrophenethylamine (2.52 g), anhydrous potassium carbonate (4.0 g) and acetonitrile (40 ml) was heated under reflux with stirring for 20 hours and then cooled and filtered. The residue was washed with acetonitrile, and the combined filtrate and washings were evaporated to give an oil which was chromarographed on silica gel. Elution with dichloromethane first gave impurity followed by pure product. The Product-containing fractions were evaporated to give the title compound (4.17 g), m.p. 76°-78° (from isopropanol).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux
  3. temperaturecooled
  4. filtrationfiltered
  5. washThe residue was washed with acetonitrile
  6. customthe combined filtrate and washings were evaporated
  7. customto give an oil which
  8. washElution with dichloromethane first gave impurity
  9. customThe Product-containing fractions were evaporated