反应详情

A mixture of Example 385C (˜18 g) in methanol (400 mL) was heated to reflux for 2 hours and then purified on a silica gel column with 20% ethyl acetate in hexanes to provide the desired product (3.95 g, 29.8% yield for three steps). 1H NMR (DMSO-d6) δ 3.90 (s, 3H), 6.22 (d, 1H), 6.60 (s, 2H), 7.30 (d, 1H), 11.70 (s, 1H); MS (DCI/NH3) m/e 246, 248 (M+H)+.

1. temperatureto reflux for 2 hours
2. custompurified on a silica gel column with 20% ethyl acetate in hexanes