反应详情

温度

80 °C

A mixture of ethyl 6-chloro-4-hydroxy-2-oxo-2′,3′,5′,6′-tetrahydro-spiro[naphthalene-1,4′-pyran]-3-carboxylate (0.810 g, 2.41 mmol), glycine methyl ester hydrochloride (0.39 g, 3.11 mmol, 1.3 eq.), 1,4-dioxane (7.0 mL) and DIPEA (1.3 mL, 7.46 mmol) was heated at 80° C. for 6 hours. The mixture was then cooled to room temperature and extracted with EtOAc (3×25 mL). The combined organic extracts were washed with 2N HCl and brine. The solution was dried (MgSO4) and concentrated under reduced pressure to give a pale yellow solid. The product was recrystallized from EtOAc to give a colorless solid (0.68 g). MS m/e=380.0 (M+H)+.

1. temperatureThe mixture was then cooled to room temperature
2. extractionextracted with EtOAc (3×25 mL)
3. washThe combined organic extracts were washed with 2N HCl and brine
4. dry with materialThe solution was dried (MgSO4)
5. concentrationconcentrated under reduced pressure
6. customto give a pale yellow solid
7. customThe product was recrystallized from EtOAc