HRID1483890

反应详情

EQUATION

反应方程式

HRID 1483890 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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-Iodopropane (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

  1. temperatureThe mixture was refluxed overnight
  2. filtrationThe reaction mixture was filtered
  3. customthe volatiles were evaporated in vacuum
  4. customThe oily residue was chromatographed on a silica column with MeOH:CH2Cl2 (1:30 (v/v)) as eluent
  5. customCollection of the fractions
  6. additioncontaining pure
  7. customproduct and evaporation of the solvent