反应详情

To a solution of 102 (1.2 g, 2.2 mmol) (Prepared according to the synthesis of Examples 151 and 152, step 1) in dichloromethane (30 mL) was added TEA (664 mg, 6.6 mmol) and MsCl (499 mg, 4.4 mmol) at 0° C. After kept 2 hours at room temperature, the reaction was quenched by water (100 mL) and extracted with dichloromethane (3×30 mL). The combined organic layer was washed with brine (20 mL) and dried over anhydrous sodium sulfate. After filtration, the filtrates were concentrated to give a residue, which was purified by silica gel column with 10%-30% ethyl acetate in petroleum ether to give the title compound (1.1 g, 80%) as brown syrup; (ES, m/z): [M+H]+ 627.0; 1H NMR (300 MHz, CDCl3) δ 7.22-7.45 (m, 15H), 6.35 (d, J=6.3 Hz, 1H), 5.03-5.15 (m, 2H), 4.61-4.80 (m, 4H), 4.47-4.53 (m, 2H), 4.25-4.36 (m, 1H), 4.08-4.12 (m, 1H), 3.89-3.92 (m, 1H), 3.46-3.78 (m, 2H), 3.06 (s, 6H), 3.01 (s, 3H).

1. customthe reaction was quenched by water (100 mL)
2. extractionextracted with dichloromethane (3×30 mL)
3. washThe combined organic layer was washed with brine (20 mL)
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationAfter filtration
6. concentrationthe filtrates were concentrated
7. customto give a residue, which
8. customwas purified by silica gel column with 10%-30% ethyl acetate in petroleum ether