HRID1972560
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
CONDITIONS
反应条件
- 温度
- 130 °C
PROCEDURE
实验过程
((2R)-1,4-dibenzyl-2-piperazinyl)methyl methanesulfonate (0.450 g, 1.202 mmol) was combined with 3-isopropylpiperazin-2-one (0.179 g, 1.262 mmol, ChemBridge, San Diego, Calif.) and potassium carbonate (0.498 g, 3.60 mmol, Sigma-Aldrich, St. Louis, Mo.) in acetonitrile (5.46 mL) and heated at 130° C. After 1 h, the mixture was diluted with EtOAc and the solids were removed by filtering through a 0.2 μm millipore Millex-FG filter (Millipore, Billerica, Mass.). After concentration, the crude residue was purified by silica gel chromatography (2.5-8.5% MeOH in CH2Cl2) to give 4-(((2R)-1,4-dibenzyl-2-piperazinyl)methyl)-3-(1-methylethyl)-2-piperazinone (212 mg).
WORKUP
后处理
- customthe solids were removed
- filtrationby filtering through a 0.2 μm
- filtrationmillipore Millex-FG filter (Millipore, Billerica, Mass.)
- concentrationAfter concentration
- customthe crude residue was purified by silica gel chromatography (2.5-8.5% MeOH in CH2Cl2)