反应详情

A mixture of Example 215 (1.0 eq) in 1,2-dimethoxyethane (10 mL) and water (5 mL) was reacted with N-[2-methoxy-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]-1-methyl-1H-indole-2-carboxamide (1.2 eq), Na2CO3 (2.4 eq), and Pd(PPh3)4 (0.06 eq) at 95° C. for 18 hours. The organic solvent was removed in vacuo and the mixture was extracted with dichloromethane. The extract was dried (MgSO4), filtered, and concentrated. The residue was purified by preparative reverse phase HPLC (Rainin C18, 8 mm, 300 Å, 25 cm; 40% acetonitrile/0.1M ammonium acetate isocratic for 5 minutes, then 40-100% acetonitrile/0.1M ammonium acetate over 30 minutes, 21 mL/min). The acetonitrile was removed in vacuo and the aqueous mixture was lyophilized to provide the desired product.

1. customThe organic solvent was removed in vacuo
2. extractionthe mixture was extracted with dichloromethane
3. dry with materialThe extract was dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified by preparative reverse phase HPLC (Rainin C18, 8 mm, 300 Å, 25 cm
7. wait40-100% acetonitrile/0.1M ammonium acetate over 30 minutes
8. customThe acetonitrile was removed in vacuo