反应详情

温度

100 °C

Methyl 3-(7-bromoimidazo[1,2-a]pyridine-3-carboxamido)-4-methylbenzoate (Intermediate 1B) (400 mg, 1.030 mmol) and TBD (143 mg, 1.030 mmol) in toluene (10 ml) was treated with (2-(4-methylpiperazin-1-yl)phenyl)methanamine (212 mg, 1.030 mmol) and heated at 100° C. under nitrogen overnight. Further TBD (106 mg, 0.82 mmol) was added the mixture was heated at 100° C. for a further 24 hrs. The solvent was removed in vacuo and the residue was partitioned between EtOAc (50 ml) and sodium bicarbonate solution (50 ml). The organic portion was separated and washed with sodium bicarbonate (2×25 ml), dried (MgSO4), filtered and evaporated to dryness to give a yellow solid. Purification by chromatography on silica eluting with 0-20% 2M NH3 in MeOH/DCM afforded a colourless oil. The oil was dissolved in minimum volume of EtOAc and titurated iso-hexane to afford the title compound as a white solid;

1. additionFurther TBD (106 mg, 0.82 mmol) was added the mixture
2. temperaturewas heated at 100° C. for a further 24 hrs
3. customThe solvent was removed in vacuo
4. customthe residue was partitioned between EtOAc (50 ml) and sodium bicarbonate solution (50 ml)
5. customThe organic portion was separated
6. washwashed with sodium bicarbonate (2×25 ml)
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. customevaporated to dryness
10. customto give a yellow solid
11. customPurification by chromatography on silica eluting with 0-20% 2M NH3 in MeOH/DCM
12. customafforded a colourless oil