反应详情

温度

100 °C

A mixture of ethyl 8-chloro-4-hydroxy-2-oxo-2′,3′,5′,6′-tetrahydro-4H-spiro[naphthalene-1,4′-pyran]-3-carboxylate (0.27 g, 0.80 mmol), and tert-butyl 2-aminoacetate hydrochloride (0.20 g, 1.2 mmol) in 1 mL dioxane was treated with N-ethyl-N-isopropylpropan-2-amine (0.26 g, 2.0 mmol). The mixture was warmed to 100° C. and stirred for 2.5 hours. The mixture was then cooled to room temperature, diluted with 20 mL H2O and 100 mL EtOAc. The organic layer was separated, dried over anhydrous sodium sulfate and concentrated. The concentrate was purified by column chromatography (10-20% EtOAc/hexane) to give 0.13 g off-white solid. MS m/e: (M+H)+ 422.

1. temperatureThe mixture was then cooled to room temperature
2. customThe organic layer was separated
3. dry with materialdried over anhydrous sodium sulfate
4. concentrationconcentrated
5. customThe concentrate was purified by column chromatography (10-20% EtOAc/hexane)