HRID542711

反应详情

EQUATION

反应方程式

HRID 542711 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of the product obtained in (a) (5 g) and N-methylpiperazine (4.3 ml) in dioxane-ethanol 9:1 (50 ml) is heated to reflux for 2 hours. After cooling and filtration of the insoluble impurities, the clear filtrate is evaporated and the residue dissolved in chloroform (100 ml). The solution is washed with a diluted ammonium hydroxyde solution (20 ml), dried, decolorized and evaporated. The residue, crystallized from methanol, yields 2.2 g of the title product, melting at 273°-275° C. (dec.).

WORKUP

后处理

  1. additionA suspension of the product
  2. temperatureis heated
  3. temperatureto reflux for 2 hours
  4. temperatureAfter cooling
  5. filtrationfiltration of the insoluble impurities
  6. customthe clear filtrate is evaporated
  7. dissolutionthe residue dissolved in chloroform (100 ml)
  8. washThe solution is washed with a diluted ammonium hydroxyde solution (20 ml)
  9. customdried
  10. customevaporated
  11. customThe residue, crystallized from methanol