反应详情

Treat a solution of (S)-tert-butyl 4-(4,5-dimethyl-6-phenylpyridazin-3-yl)-2-methylpiperazine-1-carboxylate (2.93 g, 7.66 mmol) in MeOH (20 mL) with 4 M HCl in 1,4-dioxane (10 mL, 40.0 mmol). Stir the reaction mixture at ambient temperature overnight. Concentrate the reaction mixture under reduced pressure. Dissolve the residue in MeOH, and pour onto an SCX column (Varian, 10 g). Rinse the column with MeOH. Elute the desired product with 2M NH3/MeOH. Concentrate under reduced pressure to afford the title compound (2.07 g, 95%). ES/MS m/z 283.0 (M+1).

1. concentrationConcentrate the reaction mixture under reduced pressure
2. dissolutionDissolve the residue in MeOH
3. additionpour onto an SCX column (Varian, 10 g)
4. washRinse the column with MeOH
5. washElute the desired product with 2M NH3/MeOH
6. concentrationConcentrate under reduced pressure