反应详情

温度

25 °C

A mixture comprising (2-(4-methylpiperazin-1-yl)phenyl)methanamine (413 mg, 2.010 mmol) and 5-amino-2-fluoro-4-methylbenzoic acid (step 2) (340 mg, 2.010 mmol) in DMF (3 ml) was treated with DIPEA (0.351 ml, 2.010 mmol) followed by HATU (764 mg, 2.010 mmol) and stirred at 25° C. for 24 hrs. The mixture was partitioned between water and EtOAc. The organic portion was washed with sat. aq. NaHCO3, 0.5 M LiCl and brine (each back extracted with EtOAc). The combined organic layers were dried (MgSO4), filtered and evaporated to dryness to give a pink oil. Purification by chromatography on silica eluting with 0-20% MeOH in DCM afforded the title compound;

1. customThe mixture was partitioned between water and EtOAc
2. washThe organic portion was washed with sat. aq. NaHCO3, 0.5 M LiCl and brine (each back
3. extractionextracted with EtOAc)
4. dry with materialThe combined organic layers were dried (MgSO4)
5. filtrationfiltered
6. customevaporated to dryness
7. customto give a pink oil
8. customPurification by chromatography on silica eluting with 0-20% MeOH in DCM