反应详情

Treat a solution of tert-butyl 1-(6-(4-fluorophenyl)-4,5-dimethylpyridazin-3-yl)piperidin-4-yl(methyl)carbamate (1.04 g, 2.51 mmol) in 1,4-dioxane (10 mL) with 4 M HCl in 1,4-dioxane (15.0 mL). Stir the resulting mixture at ambient temperature for 2 h. 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 and CH2Cl2, and elute the product with a 1:1 mixture of CH2Cl2 and 2 M NH3/MeOH. Concentrate under reduced pressure to afford the title compound as an off-white solid (784 mg, 99%). ES/MS m/z 315.2 (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 and CH2Cl2
5. washelute the product
6. additionwith a 1:1 mixture of CH2Cl2 and 2 M NH3/MeOH
7. concentrationConcentrate under reduced pressure