反应详情

温度

45 °C

A solution of 1-bromopentadecane (0.0051 mole) in DMF (18 ml) was added dropwise at room temperature to a mixture of intermediate (10) (0.00483 mole) and NaHCO3 (0.0051 mole) in DMF (10 ml). The mixture was stirred at 70° C. for 5 hours and at 45° C. overnight, then brought to room temperature. H2O and NaCl were added. The mixture was extracted with EtOAc. The organic layer was separated, washed with a saturated NaCl solution, dried (MgSO4), filtered and the solvent was evaporated. The residue (3.8 g) was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 98/2; 15-40 μm). The pure fractions were collected and the solvent was evaporated, yielding 0.49 g of compound 2 having a melting point of 80° C. and represented by the formula

1. custombrought to room temperature
2. extractionThe mixture was extracted with EtOAc
3. customThe organic layer was separated
4. washwashed with a saturated NaCl solution
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customthe solvent was evaporated
8. customThe residue (3.8 g) was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 98/2; 15-40 μm)
9. customThe pure fractions were collected
10. customthe solvent was evaporated