反应详情

温度

90 °C

A mixture comprising 2-tert-butoxyethanamine (1.2 g, 5.12 mmol, 50% w/w) and methyl 3-amino-4-fluorobenzoate (0.866 g, 5.12 mmol) in THF (10 ml) was treated with TBD (0.713 g, 5.12 mmol) and heated at 90° C. for 16 hrs. After cooling to RT, the solvent was removed in vacuo and the residue was partitioned between water and EtOAc. The organic portion was separated and washed with 10% aq citric acid (×2), NaHCO3 (sat. aq), brine, dried (MgSO4) and concentrated in vacuo. Purification of the crude product by chromatography on silica eluting with 0-100% EtOAc in iso-hexane afforded the title compound as a clear oil;

1. temperatureAfter cooling to RT
2. customthe solvent was removed in vacuo
3. customthe residue was partitioned between water and EtOAc
4. customThe organic portion was separated
5. washwashed with 10% aq citric acid (×2), NaHCO3 (sat. aq), brine
6. dry with materialdried (MgSO4)
7. concentrationconcentrated in vacuo
8. customPurification of the crude product by chromatography on silica eluting with 0-100% EtOAc in iso-hexane