反应详情

温度

120 °C

A mixture of K2CO3 (0.026 g, 0.19 mmol), methyl 6-cyano-7-fluoro-3,4-dihydro-2H-chromene-4-carboxylate (0.040 g, 0.17 mmol), and tert-butyl 4-hydroxy-3-methylbenzoate (0.039 g, 0.19 mmol) in 0.5 ml NMP was heated under argon at 120° C. for 24 hours. The reaction was cooled, poured into 10% aqueous HCl, and extracted with ethyl acetate. The organic extracts were dried with sodium sulfate and purified on silica gel. Elution with 25% ethyl acetate-hexanes provided material that still contained impurities. The mixture was deprotected with to 1:1 trifluoracetic acid-dichloromethane to provide the title compound (13 mg, still impure) which was used directly in the next step.

1. temperatureThe reaction was cooled
2. extractionextracted with ethyl acetate
3. dry with materialThe organic extracts were dried with sodium sulfate
4. custompurified on silica gel
5. washElution with 25% ethyl acetate-hexanes provided material that still contained impurities