反应详情

温度

0 °C

To a solution containing the product from Example 12A (1.2 g, 1.4 mmol), molecular sieves (4 Å, 6.0 g), and phosphoric acid (0.85 g) in DMF (28 mL) at 0° C. was added N-iodosuccinimide (0.406 g), and the mixture was stirred at 0° C. for 1 hour. To the cold reaction was added 10% Na2CO3 to adjust the pH to 9, and the mixture was diluted with methanol and filtered. The filtrate was treated with 1 M Na2S2O3 until it was clear, diluted with methanol and filtered again. The solvent was evaporated, and the crude product was purified by HPLC on a C18 column, eluting with a gradient starting with water and ending with methanol to give the title compound (0.605 g, 47% yield).

1. customTo the cold reaction
2. filtrationfiltered
3. additionThe filtrate was treated with 1 M Na2S2O3 until it
4. additiondiluted with methanol
5. filtrationfiltered again
6. customThe solvent was evaporated
7. customthe crude product was purified by HPLC on a C18 column
8. washeluting with a gradient