HRID2119361
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
1-(3,3-Diphenylpropyl)homopiperazine (2.0 g, 6.79 mmol) was dissolved in CH3CN (60 mL) and treated with methyl bromoacetate (1.56 g, 10.18 mmol) and Et3N (1.42 mL, 10.18 mmol). The mixture was refluxed for 18 h and subsequently concentrated in vacuo. The residue was subjected to flash silica gel column chromatography (eluent: CH2Cl2/MeOH, 96/4, v/v) to give Methyl [4-(3,3-diphenylpropyl)homopiperazine-1-yl]acetate (1.93 g) in 78% yield, TLC Rf=0.53 (10% CH3OH—CH2Cl2); RPLC tR=4.71 min (>85%), 220 nm (Method A); ESI/MS m/e 367.1 (M++H, C23H30N2O2).
WORKUP
后处理
- temperatureThe mixture was refluxed for 18 h
- concentrationsubsequently concentrated in vacuo