反应详情

To a solution of tris(1,1-dimethylethyl)2-{2-chloro-6-[(2R)-2,4-dimethyl-1-piperazinyl]-5-fluoro-4-pyrimidinyl}-1,1,2-hydrazinetricarboxylate (215.28 g, 374.3 mmol) in DCM (1870 mL) was added 2 N HCl in Et2O (1870 mL, 3740 mmol). The solution was mechanically stirred for 64 h, and the resulting suspension was allowed to settle. Most of the solvent was then decanted, and the remaining solid was triturated with DCM (1000 mL) and collected by vacuum filtration. The solid was washed with DCM and dried under high vacuum to provide 2-chloro-4-[(2R)-2,4-dimethyl-1-piperazinyl]-5-fluoro-6-hydrazinopyrimidine, assumed trihydrochloride (138.22 g, 96% yield) as a light yellow powder. LCMS: (M+H)+: 275.1.

1. customMost of the solvent was then decanted
2. customthe remaining solid was triturated with DCM (1000 mL)
3. filtrationcollected by vacuum filtration
4. washThe solid was washed with DCM
5. customdried under high vacuum