反应详情

To a solution of methyl imidazo[1,2-a]pyridine-7-carboxylate (1 g, 5.68 mmol) in DMF (30 ml) was added N-iodosuccinimide (1.53 g, 1.2 equiv) and the resulting mixture was stirred for 2 h at room temperature. The thin brown slurry was diluted with water, 10% w/v sodium thiosulfate and sodium carbonate (1M) and extracted with CH2Cl2. The aqueous was further extracted with CH2Cl2. The combined organic phases were washed with brine (280 ml), dried (MgSO4) and concentrated in vacuo to give a brown residue. The residue was triturated with ether, filtered and the solid was washed ether (2×50 ml) and dried on the filter to give the product as a white solid (0.81 g). 1H NMR (400 MHz, Me-d3-OD): 8.44 (1H, d), 8.25 (1H, s), 7.88 (1H, s), 7.61 (1H, dd), 3.95 (3H, s). MS: [M+H]+ 303.

1. extractionextracted with CH2Cl2
2. extractionThe aqueous was further extracted with CH2Cl2
3. washThe combined organic phases were washed with brine (280 ml)
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. customto give a brown residue
7. customThe residue was triturated with ether
8. filtrationfiltered
9. washthe solid was washed ether (2×50 ml)
10. customdried on the
11. filtrationfilter