反应详情

A solution of 33-1 (10 g, 42.7 mmol) in THF (50 mL) was treated with 1N LiOH (47 mL, 47.0 mmol) and water (50 mL). The resulting solution was stirred at ambient temperature for 12 h. The solution was concentrated and the aqueous residue was cooled to 0° C., then adjusted to pH=6 with 1N HCl. The resulting solid was collected by filtration and dried in vacuo to afford 33-2 as a white solid. 1H NMR (D2O) δ 7.95 (d, J=6.8 Hz, 2HO, 6.73 (d, J=6.8 Hz, 2h), 3.76 (d, J=12.8 Hz, 2HO, 2.81 (m, 2H), 2.20 (m, 1H), 1.85 (d, J=12.9 Hz, 2H), 1.55 (m, 2H). ##STR165## Ethyl 4-(Pyridyl)(piperidin-4-yl)-carbonylamino-3-methylphenoxyacetate (33-3)

1. concentrationThe solution was concentrated
2. temperaturethe aqueous residue was cooled to 0° C.
3. filtrationThe resulting solid was collected by filtration
4. customdried in vacuo