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17th May 2013 @ 10:19
Repeat of [blog=7410]Nucleophilic Displacement of MNR99 with 1-Methylpiperazine to give MNR125-1[/blog] but with 1.5 equiv of amine rather than 2. Procedure: To MNR 99-3 (1.0 g, 5.86 mmol, 1 equiv)) in THF (7 mL) (ethanol (5 mL added to get the starting material into solution) was added 1-methylpiperazine (0.98 mL, 8.79 mmol, 1.5 equiv) at 0 ˚C and the reaction mixture was stirred overnight at room temperature. Volatiles removed in vacuo (~4 mL remains) and then dissolved in EtOAc, washed with a saturated aqueous solution of sodium hydrogen carbonate, water, brine, dried (MgSO4), filtered and evaporated to give a Data: TLC 20 h 100% EtOAc [data]6448[/data] Hazard and Risk Assessment: See [blog=7410]Nucleophilic Displacement of MNR99 with 1-Methylpiperazine to give MNR125-1[/blog] and links within.    
Attached Files
AEW 55-1.png
AEW 54 and 55 100% EtOAc.jpg