反应详情

温度

80 °C

To a solution of (50) from Example 17 (3.6 g, 9.7 mmol) in dry THF (20 ml) was added 5-acetyl-1-(3-bromophenyl)benzimidazole (52) (1.5 g, 4.8 mmol) and (PPh3)2PdCl2 (340 mg, 0.48 mmol) under argon. The reaction mixture was stirred at 80° C. for 24 hr in a 50 ml sealed tube. After cooling the mixture was concentrated, triturated with water (100 ml) and extracted with CH2Cl2 (200 ml×3). The extract was washed with brine, dried and concentrated under reduced pressure. The residue was washed with ether to afford crystalline (51) (1.5 g, 89%).

1. customsealed tube
2. temperatureAfter cooling the mixture
3. concentrationwas concentrated
4. customtriturated with water (100 ml)
5. extractionextracted with CH2Cl2 (200 ml×3)
6. washThe extract was washed with brine
7. customdried
8. concentrationconcentrated under reduced pressure
9. washThe residue was washed with ether