反应详情

温度

55 °C

A slurry of 2,4-dihydroxy actophenone (3.8 g; 25 mmol) and KHCO3 (2.75 g; 27.5 mmol) in DMF (50 mL) was stirred at 50° C. for 1 hour and then added 1-bromooctane (4.75 mL; 27.5 mmol). The reaction mixture was stirred at 50-60° C. for 7 days, poured onto H2O (100 mL) and the aqueous phase extracted with diethyl ether (3×). The combined organic fractions was dried (MgSO4), filtered, evaporated to dryness and purified by column chromatography (SiO2; EtOAc/PE80-100° C.=1:10) to yield 4.39 g (66%) as yellow oil. MS (direct; Cl): 265 (MH+).

1. additionpoured onto H2O (100 mL)
2. extractionthe aqueous phase extracted with diethyl ether (3×)
3. dry with materialThe combined organic fractions was dried (MgSO4)
4. filtrationfiltered
5. customevaporated to dryness
6. custompurified by column chromatography (SiO2; EtOAc/PE80-100° C.=1:10)
7. customto yield 4.39 g (66%) as yellow oil