反应详情

Add 2-chloro-N-(3-fluoro-4-nitro-phenyl)pyridin-4-amine (300 mg, 1.12 mmol), methyl iodide (174 mg, 1.23 mmol) and K2CO3 (201 mg, 1.45 mmol) in DMF (6 mL). Stir the reaction at 70° C. for 3 hrs. TLC (EtOAc:PE=1:1) shows the reaction is complete, cool the reaction to 0° C., add water, extract with EtOAc. Combine the organic layers. Wash with brine, dry over anhydrous Na2SO4. Concentrate to give the crude product. Purification by chromatography (silica gel, EtOAc:PE=1:1) affords the title compound (190 mg, 45%). MS: (M+1): 282.2.

1. customthe reaction at 70° C. for 3 hrs
2. temperaturecool
3. customthe reaction to 0° C.
4. extractionextract with EtOAc
5. washWash with brine
6. dry with materialdry over anhydrous Na2SO4
7. concentrationConcentrate
8. customto give the crude product
9. customPurification by chromatography (silica gel, EtOAc:PE=1:1)