反应详情

A suspension of 131 (30 mg, 0.09 mmol) and diethoxymethyl acetate (1 mL) is stirred at room temperature for 10 minutes. NaHCO3 (aq.) (10 mL) and dichloromethane (10 mL) are added. The organic layer is separated and the aqueous layer is extracted with dichloromethane (2×10 mL). The combined organic layers are dried (NaSO4) and solvent removed. The crude product is separated by PTLC (10% methanol in dichloromethane) to yield 187; LC-MS, M+1 338.15; 1H-NMR (CDCl3) δ: 8.87 (s, 1H), 8.83 (s, 1H), 8.42 (s, 1H), 7.54 (t, 1H), 7.23–7.34 (m, 3H), 5.79 (s, 2H), 3.02 (t, 2H), 1.66–1.76 (m, 2H), 0.99 (t, 3H).

1. customThe organic layer is separated
2. extractionthe aqueous layer is extracted with dichloromethane (2×10 mL)
3. dry with materialThe combined organic layers are dried (NaSO4) and solvent
4. customremoved
5. customThe crude product is separated by PTLC (10% methanol in dichloromethane)