反应详情

To a vigorously stirred solution of isopropyl amine (83 μL, 1.21 mmol) in DMF (6 mL) at 0° C. was added DIPEA (0.24 mL, 1.33 mmol) followed immediately by tris(1,1-dimethylethyl)2-(2,6-dichloro-5-fluoro-4-pyrimidinyl)-1,1,2-hydrazinetricarboxylate (600 mg, 1.21 mmol). When the reaction was complete as determined by LCMS, the reaction mixture was diluted with diethyl ether (˜40 mL) and washed with water (3×40 mL). The combined three aqueous layers were back-extracted once with diethyl ether, and then the combined organics were dried (Na2SO4) and concentrated in vacuo. This crude product was purified by flash chromatography (Combiflash, 5-60% ethyl acetate/hexanes, 1% triethylamine) to provide tris(1,1-dimethylethyl)2-{2-chloro-5-fluoro-6-[(1-methylethyl)amino]-4-pyrimidinyl}-1,1,2-hydrazinetricarboxylate (597 mg, 95%). LCMS: (M+H)+: 520.2.

1. washwashed with water (3×40 mL)
2. extractionwere back-extracted once with diethyl ether
3. dry with materialthe combined organics were dried (Na2SO4)
4. concentrationconcentrated in vacuo
5. customThis crude product was purified by flash chromatography (Combiflash, 5-60% ethyl acetate/hexanes, 1% triethylamine)