反应详情

4M HCl in dioxane solution (8 ml) was added in one portion to a stirred solution of 4-[6-(3,4-Dichloro-phenyl)-pyrimidin-4-yl]-piperazine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester (0.36 g, 0.75 mmol) in dioxane (2 ml) and the mixture was stirred at room temperature overnight. After this time the reaction mixture was concentrated and the resulting residue was partitioned between DCM (100 ml) and saturated sodium bicarbonate (75 ml) and stirred at room temperature for 10 minutes. The mixture was then extracted with DCM (3×100 ml), the organic layers were combined, separated and washed with brine (50 ml). The organic layer was removed, dried (MgSO4) filtered and concentrated to give the title compound (0.27 g, 87% yield) as a yellow solid.

1. concentrationAfter this time the reaction mixture was concentrated
2. customthe resulting residue was partitioned between DCM (100 ml) and saturated sodium bicarbonate (75 ml)
3. stirringstirred at room temperature for 10 minutes
4. extractionThe mixture was then extracted with DCM (3×100 ml)
5. customseparated
6. washwashed with brine (50 ml)
7. customThe organic layer was removed
8. dry with materialdried (MgSO4)
9. filtrationfiltered
10. concentrationconcentrated