HRID1024950

反应详情

EQUATION

反应方程式

HRID 1024950 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 1-Methylpiperazine (1.58 g) in dioxane was added sulfamide (4.0 g) and the reaction mixture was then heated at reflux in dioxane for 18 h. The reaction mixture was then reduced in vacuo and the residue partitioned between EtOAc (100 ml) and H2O (100 ml). The organics were separated and the aqueous layer was re-extracted with EtOAc (2×100 ml). Organics were combined, dried (MgSO4) and reduced in vacuo to give the subtitle compound as a white solid. Yield: 640 mg

WORKUP

后处理

  1. temperaturethe reaction mixture was then heated
  2. customthe residue partitioned between EtOAc (100 ml) and H2O (100 ml)
  3. customThe organics were separated
  4. extractionthe aqueous layer was re-extracted with EtOAc (2×100 ml)
  5. dry with materialdried (MgSO4)