反应详情

温度

90 °C

A mixture of the allylic alcohol of Example 1, Step 11, (30.14 g, 121 mmol), 1,2-dibromobenzene (16 mL), Pd(OAc)2 (830 mg), LiCl (5.38 g), LiOAc.2H2O (31.6 g), and Bu4NCl (67.96 g) in 240 mL of DMF was degassed and heated to 85° C. under N2 for 30 min and at 90° C. for 45 min. It was then added to ice and 25% aq. NH4OAc (2 L). The title ketone was extracted in EtOAc, dried over Na2SO4 and purified by flash chromatography on silica with EtOAc:hexane 10:90; yield: 29.53 g (60%).

1. customwas degassed
2. additionIt was then added to ice and 25% aq. NH4OAc (2 L)
3. extractionThe title ketone was extracted in EtOAc
4. dry with materialdried over Na2SO4
5. custompurified by flash chromatography on silica with EtOAc:hexane 10:90