反应详情

To a stirred solution of 2-methylpiperazine (10.0 g, 0.1 mol) in dry CH2Cl2 (500 ml) under argon was added a solution of 1.0 M Me2AlCl or Et2AlCl in hexanes (100 ml, 0.1 mmol) and methyl benzoate (12.4 ml, 0.1 mmol) at room temperature. The reaction mixture was then stirred for 2 days before 2N NaOH (200 ml) was added. Aqueous layer was extracted with EtOAc (3×100 ml). The combined organic layer was dried over MgSO4 and concentration of solution provided 20.0 g of crude product (98%), with was pure enough for the further reactions.

1. additionwas added
2. extractionAqueous layer was extracted with EtOAc (3×100 ml)
3. dry with materialThe combined organic layer was dried over MgSO4 and concentration of solution