反应详情

MsCl (3.3 g, 28 mmol) and Et3N (3.8 g, 38 mmol) were added to a mixture of 1-(2,4-dimethoxybenzyl)-4-(1-hydroxyethyl)pyrrolidin-2-one (5.0 g, 19 mmol) in dichloromethane (50 mL) at 0° C. The mixture was stirred at room temperature for 10 hours then diluted with water and extracted with EtOAc. The EtOAc layer was dried over sodium sulfate and concentrated under reduced pressure to afford 1-[1-(2,4-dimethoxybenzyl)-5-oxopyrrolidin-3-yl]ethyl methanesulfonate. 1H NMR (400 MHz, CDCl3) δ 7.10˜7.13 (m, 1H), 6.43-6.45 (m, 2H), 4.76-4.78 (m, 1H), 4.41-4.42 (m, 2H), 3.79-3.82 (m, 6H), 3.36-3.42 (m, 1H), 3.12-3.19 (m, 1H), 2.98 (s, 3H), 2.23-2.59 (m, 3H), 1.26-1.42 (d, J=7.2 Hz, 3H). MS ESI calc'd. for C16H24NO6S [M+H]+ 358. found 358.

1. extractionextracted with EtOAc
2. dry with materialThe EtOAc layer was dried over sodium sulfate
3. concentrationconcentrated under reduced pressure