HRID2181589

反应详情

EQUATION

反应方程式

HRID 2181589 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of p-xylenediamine (2.0 g) in dichloromethane (200 ml) maintained below 10° C. was added N,N-diisopropylamine (2.52 ml) followed by the dropwise addition of acetylchloride (1.15 g). The mixture was allowed to attain room temperature and stirred overnight. Water (120 ml) was added and the suspension filtered. The filtered solid was washed with dichloromethane (2×100 ml) and water (100 ml). All filtrates were combined and the organic layer separated. The organic layer was washed with water, dried (MgSO4) and evaporated to give the title product as a solid, m.p. 133-5° C.

WORKUP

后处理

  1. customto attain room temperature
  2. filtrationthe suspension filtered
  3. washThe filtered solid was washed with dichloromethane (2×100 ml) and water (100 ml)
  4. customthe organic layer separated
  5. washThe organic layer was washed with water
  6. dry with materialdried (MgSO4)
  7. customevaporated