反应详情

温度

80 °C

A mixture comprising 2-(2,6-cis-dimethylpiperidin-1-yl)ethanaminium chloride (4 g, 20.75 mmol) and methyl 3-amino-4-fluorobenzoate (3.51 g, 20.75 mmol) in THF (50 ml) was treated with TBD (2.89 g, 20.75 mmol) and stirred at 80° C. for 16 hrs. A further portion of methyl 3-amino-4-fluoro benzoate (1 g) and TBD (0.5 g) were added and heating continued for 24 hrs. The resulting mixture was partitioned between ethyl acetate and aqueous sodium bicarbonate. The mixture was extracted once with ethyl acetate and once with chloroform. The combined organic layers were dried (MgSO4), filtered and evaporated to dryness. Purification of the residue by chromatography on silica eluting with 0-20% MeOH in DCM afforded the title compound;

1. temperatureheating
2. waitcontinued for 24 hrs
3. customThe resulting mixture was partitioned between ethyl acetate and aqueous sodium bicarbonate
4. extractionThe mixture was extracted once with ethyl acetate and once with chloroform
5. dry with materialThe combined organic layers were dried (MgSO4)
6. filtrationfiltered
7. customevaporated to dryness
8. customPurification of the residue by chromatography on silica eluting with 0-20% MeOH in DCM