反应详情

温度

80 °C

1,1-dimethylethyl {[3-bromo-5-(methyloxy)phenyl]methyl}carbamate (1.4 g, 4.43 mmol), Pd(OAc)2 (70.0 mg, 0.14 mmol), dicyclohexyl[2′-(methyloxy)-1,1′-binaphthalen-2-yl]phosphane (84.0 mg, 0.175 mmol) and K3PO4 (1.2 g, 5.31 mmol) were dissolved in dioxane (30 mL). The mixture was heated at 80° C. for 30 min, and then [3-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)phenyl]boronic acid (1.5 g, 5.76 mmol) was added. The mixture reaction was stirred at reflux for two days. The solvent was removed under reduced pressure, then the residue diluted with CH2Cl2 (100 mL). The organic layer was washed with water (20 mL), brine (20 mL), and dried over Na2SO4. The product 1,1-dimethylethyl[3′-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)-5-(methyloxy)-3-biphenylyl]methyl}carbamate (1.5 g) was purified by flash column chomatography (PE:EA=15:1) (yield: 74%).

1. customThe mixture reaction
2. temperatureat reflux for two days
3. customThe solvent was removed under reduced pressure
4. additionthe residue diluted with CH2Cl2 (100 mL)
5. washThe organic layer was washed with water (20 mL), brine (20 mL)
6. dry with materialdried over Na2SO4
7. customThe product 1,1-dimethylethyl[3′-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)-5-(methyloxy)-3-biphenylyl]methyl}carbamate (1.5 g) was purified by flash column chomatography (PE:EA=15:1) (yield: 74%)