反应详情

A mixture of Example 60 (17 mg, 0.04 mmol), acetyl chloride (3.2 mg, 0.4 mmol) and pyridine (0.5 mL, 0.8 mmol) in THF (10 mL) was stirred at r.t. for 2 days. It was concentrated in vacuo and purified by preparative HPLC (Method 7) to give the title compound (8.8 mg, 47%) as an off-white solid. δH (CDCl3) 8.53-8.34 (1H, m), 8.31-8.18 (1H, m), 7.60-7.51 (1H, m), 7.24-7.11 (1H, m), 7.03-6.88 (2H, m), 5.23 (1H, br s), 4.47-4.28 (2H, m), 4.14-3.98 (2H, m), 2.94-2.80 (2H, m), 2.63-2.48 (3H, m), 2.27-2.07 (3H, m), 1.40 (6H, s). LCMS (ES+) 464 (M+H)+, RT 2.70 minutes (Method 2).

1. concentrationIt was concentrated in vacuo
2. custompurified by preparative HPLC (Method 7)