米诺地尔杂质22

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Piperidine (25.67 g, 0.0302 m) is added dropwise to an ice-cooled solution of 41.36 g (0.0302 m) of ethyl N, 2-dicyanoacetimidate in 60 ml of methanol. The reaction is heterogeneous initially, but soon becomes homogeneous and yellow. The piperidine is added at a rate that maintains a 25° C. reaction temperature. After fifty minutes, the reaction mixture is partitioned between CH2Cl2 and aqueous saturated NaHCO3. The organic phase is dried over Na2SO4 and concentrated in vacuo to give 54 g of a yellow oil which by tlc appears to be pure product. Nmr confirms the presence of product. that maintains a 25° C. reaction temperature After fifty minutes the reaction mixture is partitioned between CH2Cl2 and aqueous saturated NaHCO3 The organic phase is dried over Na2SO4 concentrated in vacuo

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Piperidine (25.67 g, 0.0302 m) is added dropwise to an ice-cooled solution of 41.36 g (0.0302 m) of ethyl N, 2-dicyanoacetimidate in 60 ml of methanol. The reaction is heterogeneous initially, but soon becomes homogeneous and yellow. The piperidine is added at a rate that maintains a 25° C. reaction temperature. After fifty minutes, the reaction mixture is partitioned between CH2Cl2 and aqueous saturated NaHCO3. The organic phase is dried over Na2SO4 and concentrated in vacuo to give 54 g of a yellow oil which by tlc appears to be pure product. Nmr confirms the presence of product. that maintains a 25° C. reaction temperature After fifty minutes the reaction mixture is partitioned between CH2Cl2 and aqueous saturated NaHCO3 The organic phase is dried over Na2SO4 concentrated in vacuo