反应详情

To a stirred solution of 66.15C (1.00 g, 3.6 mmol) in DME (10.00 mL, 96 mmol) at 23° C. was added sulfuric acid (0.19 mL, 3.6 mmol) in water (8 mL), followed by dropwise addition of a solution of sodium nitrite (0.38 g, 5.4 mmol) in water (2 mL) at 0° C. over 30 minutes. The reaction was then stirred for 20 minutes. To the mixture was added a solution of sodium iodide (3.0 g, 20 mmol) in water (7 mL) at 0° C. The resulting mixture was then stirred for 1 hour. The reaction was quenched with sodium thiosulfate and extracted three times with diethyl ether. After drying over anhydrous magnesium sulfate and filtering, the organic solvent was removed under reduced pressure and the product was purified on silica gel (0-40% EtOAc in hexanes) to yield a colorless solid 66.15D (0.820 g, 58% yield).

1. stirringThe resulting mixture was then stirred for 1 hour
2. customThe reaction was quenched with sodium thiosulfate
3. extractionextracted three times with diethyl ether
4. dry with materialAfter drying over anhydrous magnesium sulfate
5. filtrationfiltering
6. customthe organic solvent was removed under reduced pressure
7. customthe product was purified on silica gel (0-40% EtOAc in hexanes)