反应详情

2-Methyl-2-(3-piperidin-3-yl-phenoxy)-propionic acid methyl ester (4.80 g, 17.31 mmol) was dissolved in THF (80 mL) and followed by the addition of L-(+)-tartaric acid (2.86 g, 19.04 mmol). The resulting mixture was refluxed under nitrogen for 3 h. While the mixture was still hot, the solid was collected by vacuum-filtration, rinsed with THF, and further dried to afford 7.13 g (96%) of 2-methyl-2-(3-piperidin-3-yl-phenoxy)-propionic acid methyl ester tartrate salt as a white solid: 1H NMR (DMSO-d6) δ 1.50 (s, 6H), 1.60–1.73 (m, 2H), 1.83 (d, 2H), 2.80–2.94 (m, 3H), 3.24 (d, 2H), 3.67 (s, 3H), 3.87 (s, 2H), 6.60 (d, 1H), 6.69 (s, 1H), 6.89 (d, 1H), 7.21 (t, 1H); MS m/z (relative intensity) 277 (M+, 2), 218 (6), 176 (100).

1. temperatureThe resulting mixture was refluxed under nitrogen for 3 h
2. filtrationthe solid was collected by vacuum-filtration
3. washrinsed with THF
4. customfurther dried