反应详情

温度

0 °C

To a solution containing the product from Example 13A (0.888 g, 1.03 mmol), molecular sieves (4 Å, 3.5 g), and phosphoric acid (0.50 g) in DMF (20 mL) at 0° C. was added N-iodosuccinimide (0.46 g), and the mixture was stirred at 0° C. for 1 hour. To the cold reaction mixture was added 10% Na2CO3 to adjust the pH to 9, and the mixture was diluted with methanol, treated with 1 M Na2S2O3 until it was clear, and filtered to remove the solids. The solvent was evaporated, and the crude product was purified by HPLC using C18 column, eluting with a gradient starting with water and ending with methanol to give the product (0.49 g, 52% yield). 1H NMR (300 MHz, MeOH-d4), δ ppm 0.86-1.03 (m, 12H), 1.33-1.36 (m, 6H), 1.44-1.75 (m, 1H), 1.85-2.27 (m, 3H), 2.54-2.9 (m, 5H), 3.01 (s, 3H), 3.78-4.38 (m, 4H), 4.46-4.68 (m, 2H), 4.91-5.15 (m, 3H), 6.97-7.26 (m, 11H), 7.64-7.73 (m, 1H), 8.91-8.92 (m, 1H).

1. customTo the cold reaction mixture
2. filtrationfiltered
3. customto remove the solids
4. customThe solvent was evaporated
5. customthe crude product was purified by HPLC
6. washeluting with a gradient