反应详情

温度

80 °C

1-(2-Hydroxyethyl)-4-(4-nitrophenyl)piperazine (5 g, 0.02 mol) was dissolved in 50 mL of DCM and treated with HCl (40 mL of a 1M solution in Et2O) under a drying tube for 90 min. The solvent was evaporated, the residue dissolved in thionyl chloride (60 mL) and the mixture refluxed at 80° C. After 5 h, the reaction was complete as shown by LCMS and the thionyl chloride was removed under reduced pressure redissolving in DCM and evaporating three times to give the title compound as the HCl salt. LCMS: 93%, t=0.88 min, [MH+]=270.23.

1. customThe solvent was evaporated
2. dissolutionthe residue dissolved in thionyl chloride (60 mL)
3. customthe thionyl chloride was removed under reduced pressure
4. dissolutionredissolving in DCM
5. customevaporating three times