反应详情

To a degassed solution of the product of step 1 (5.7 g, 24.2 mmol,), and 4-hydroxymethylphenylboronic acid (5.47 g, 36 mmol) in toluene (150 mL) was added Pd2(dba)3 (1.09 g, 1.2 mmol). The mixture was degassed and Ph3P (2.5 g, 9.6 mmol), Et2NH (2.63 g, 36 mmol), n-propanol (18 mL) and H2O (18 mL) was added. The mixture was heated to reflux for 26 h. Aqueous NaHCO3 was added and the resulting mixture was extracted with EtOAc. The combined organic extracts were washed with brine, dried (anhyd. MgSO4) and concentrated in vacuo. The residue was purified by chromatography on silica gel to give 6.06 g (95%) of the title compound.

1. customThe mixture was degassed
2. temperatureThe mixture was heated
3. temperatureto reflux for 26 h
4. extractionthe resulting mixture was extracted with EtOAc
5. washThe combined organic extracts were washed with brine
6. dry with materialdried (anhyd. MgSO4)
7. concentrationconcentrated in vacuo
8. customThe residue was purified by chromatography on silica gel