反应详情

温度

70 °C

A solution was prepared of 9.8 g (35 mmol) of 1-hydroxy-2-(3-methoxyphenyl)-6-methoxynaphthalene in 490 mL of DMF under a nitrogen atmosphere and to this solution was slowly added 1.47 g (36.8 mmol) of 60% NaH in mineral oil. After ten minutes, 7.5 mL (70 mmol) of 4-fluorobenzaldehyde was added and the reaction mixture was heated to 70° C. for sixty-four hours. The reaction mixture was evaporated to dryness and the residue partitioned between water and EtOAc. The EtOAc layer was dried with Na2SO4 and chromatographed on a silica gel column eluted with EtOAc-hexane (1:9)(v/v). The final product was further purified by crystallization from MeOH. This yielded 2.4 g of the title compound as a tan solid, mp 145-146° C.

1. waitAfter ten minutes
2. customThe reaction mixture was evaporated to dryness
3. customthe residue partitioned between water and EtOAc
4. dry with materialThe EtOAc layer was dried with Na2SO4
5. customchromatographed on a silica gel column
6. washeluted with EtOAc-hexane (1:9)(v/v)
7. customThe final product was further purified by crystallization from MeOH