反应详情

To a solution of N-methoxy-N-methyl-1H-indazole-3-carboxamide (12.4 g, 60.42 mmol) in CH2Cl2 (200 mL) was added bis(trifluoroacetoxy)iodobenzene (28.78 g, 66.74 mmol), followed by dropwise addition of iodine (9.22 g, 36.33 mmol) in CH2Cl2 at rt. The reaction was stirred overnight, after which 300 mL saturated NaHSO3 was added and a solid began to precipitate, which was then filtered. The filtrate was concentrated and triturated with a small amount of CH2Cl2. The combined solids were dried to give 5-iodo-N-methoxy-N-methyl-1H-indazole-3-carboxamide (14.4 g, 72%) as a yellow solid.

1. customto precipitate
2. filtrationwhich was then filtered
3. concentrationThe filtrate was concentrated
4. customtriturated with a small amount of CH2Cl2
5. customThe combined solids were dried