反应详情

温度

95 °C

To the suspension solution of 2-[(2-chloro-5-fluoro-4-pyrimidinyl)amino]-N-(1-methylethyl)benzamide (100 mg, 0.32 mmol) and (5R)-1-(3-aminophenyl)-5-methyl-4-(trifluoroacetyl)-2-piperazinone (147 mg, 0.48 mmol) was added 2 drops of 12N HCl. The reaction mixture was then sealed and heated in a 95° C. oil bath for 16 h. The reaction was followed by LC/MS. The reaction was evaporated to dryness. The residue was then dissolved in THF (10 mL) with LiOH (1.0 M solution 0.64 mL). The reaction mixture was heated at 50° C. for 3 h. Then the solvent was evaporated to dryness on high vacuum and the residue was loaded on silica gel column and eluted with 2.0 to 9.0% MeOH (with 0.1% NH4OH) in CH2Cl2. Oil was then recrystalized from hot EtOH to yield the pure title compound (84 mg, 55%). MS: M(C25H28FN7O2)=477.54 (M+H)+=478.

1. customThe reaction mixture was then sealed
2. customThe reaction was evaporated to dryness
3. dissolutionThe residue was then dissolved in THF (10 mL) with LiOH (1.0 M solution 0.64 mL)
4. temperatureThe reaction mixture was heated at 50° C. for 3 h
5. customThen the solvent was evaporated to dryness on high vacuum
6. washeluted with 2.0 to 9.0% MeOH (with 0.1% NH4OH) in CH2Cl2
7. customOil was then recrystalized from hot EtOH