HRID1175456
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe reaction mixture was then heated
- customthe residue partitioned between EtOAc (100 ml) and H2O (100 ml)
- customThe organics were separated
- extractionthe aqueous layer was re-extracted with EtOAc (2×100 ml)
- dry with materialdried (MgSO4)