反应详情

A solution of 1,8-diiodonaphthalene, (1.70 g, 4.5 mmol), 2-methyl-4-methoxyphenylboronic acid, 2, (2.20 g, 13.4 mmol), Pd(PPh3)4 (0.78 g, 0.67 mmol) and K3PO4, (4.30 g, 20.1 mmol) in 50 mL toluene was stirred at 100° C. for 18 hours. The resulting mixture was allowed to come to room temperature, quenched with water and extracted with CH2Cl2. The combined organic layers were dried over MgSO4 and concentrated in vacuo. Purification by flash chromatography on silica gel (CH2Cl2:hexanes 2:3) afforded 1.65 g (4.5 mmol, >99%) of off-white crystals containing syn- and anti-isomers of 7 in a ratio of 1:3.

1. customto come to room temperature
2. customquenched with water
3. extractionextracted with CH2Cl2
4. dry with materialThe combined organic layers were dried over MgSO4
5. concentrationconcentrated in vacuo
6. customPurification by flash chromatography on silica gel (CH2Cl2:hexanes 2:3)