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
A suspension of 1-(3-methanesulfonyl-phenyl)piperazine (350 mg) and ground K2CO3 (403 mg) was stirred in CH3CN (25 mL) at room temperature. 1-Iodo-propane (712 μL) was added. The mixture was refluxed overnight. The reaction mixture was filtered and the volatiles were evaporated in vacuum. The oily residue was chromatographed on a silica column with MeOH:CH2Cl2 (1:30 (v/v)) as eluent. Collection of the fractions containing pure product and evaporation of the solvent afforded pure 1-(3-methanesulfonyl-phenyl)-4-propyl-piperazine (220 mg). The amine was converted into the HCl salt and recrystallized from ethanol/diethylether: m.p. 233° C. MS m/z (relative intensity, 70 eV) 282 (M+, 30), 254 (15), 253 (bp), 210 (17), 70 (21).
WORKUP
后处理
- temperatureThe mixture was refluxed overnight
- filtrationThe reaction mixture was filtered
- customthe volatiles were evaporated in vacuum
- customThe oily residue was chromatographed on a silica column with MeOH:CH2Cl2 (1:30 (v/v)) as eluent
- customCollection of the fractions
- additioncontaining pure
- customproduct and evaporation of the solvent