HRID1181853

反应详情

EQUATION

反应方程式

HRID 1181853 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a mixture of potassium phosphate (8.36 g 40 mmol), palladium acetate (0.88 g, 0.4 mmol), 2-(dicyclohexylphosphino)biphenyl (0.54 g, 1.6 mmol) and nphthalene-2-boronic acid (5.09 g, 30 mmol) was added 3-cloro-2-methyl-biphenyl (4.0 g, 20 mmol). The reaction mixture was heated to 80° C. overnight, diluted with diethyl ether, washed with water and dried over MgSO4. Removal of solvent under reduced pressure gave a crude product that was purified by silica gel chromatography eluting with hexanes gave 2-(2-methyl-1,1′-biphenyl-3-yl)naphthalene as a white solid; mp 106-107° C.; MS (EI) m/z 294.17 (M+); 1H NMR (CDCl3): δ 2.15 (s, 3H), 7.20-7.55 (m, 11H), 7.75-7.90 (m, 4H); Anal. Calcd for C23H18: C, 93.84; H, 6.16. Found: C, 93.81; H, 5.95.

WORKUP

后处理

  1. washwashed with water
  2. dry with materialdried over MgSO4
  3. customRemoval of solvent under reduced pressure
  4. customgave a crude product that
  5. customwas purified by silica gel chromatography
  6. washeluting with hexanes