HRID467107
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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 chromatographed 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
- temperaturewas heated
- temperatureunder reflux
- temperaturecooled
- filtrationfiltered
- washThe residue was washed with acetonitrile
- customthe combined filtrate and washings were evaporated
- customto give an oil which
- customwas chromatographed on silica gel
- washElution with dichloromethane first gave impurity
- customThe product-containing fractions were evaporated