反应详情

In a round-bottomed flask, 5-(tert-butyl-dimethyl-silanyloxy)-1H-indazole (1.20 g, 4.83 mmol) was dissolved in DMF (12 ml). Iodine (2.45 g, 9.66 mmol) was added followed by potassium carbonate (2.58 g, 18.7 mmol). The dark suspension was stirred at room temperature for 3 h then quenched with 10% aqueous NaHSO3 and extracted with diethyl ether (2×). The combined organic layers were washed with 10% aqueous NaHSO3, three times with water and once with brine then dried over sodium sulfate, filtered and concentrated to afford 1.65 g (91%) of 5-(tert-butyl-dimethyl-silanyloxy)-3-iodo-1H-indazole as a dark brown foam.

1. customthen quenched with 10% aqueous NaHSO3
2. extractionextracted with diethyl ether (2×)
3. washThe combined organic layers were washed with 10% aqueous NaHSO3, three times with water and once with brine
4. dry with materialthen dried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated