反应详情

To a stirred solution of 7-chloro-6-fluoro-5-hydroxy-3,4-dihydro-2H-naphthalen-1-one (0.90 g, 4.18 mmol) in dry N,N-dimethylformamide (10 mL) was added potassium carbonate (1.16 g, 8.36 mmol) and tert-butyl bromoacetate (1.22 g, 6.27 mmol) at room temperature and the resulting mixture was stirred for 2 hours, then extracted with ethyl acetate (25 mL×3), washed with water (25 mL×3), dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo to afford (3-chloro-2-fluoro-5,6,7,8-tetrahydro-naphthalen-1-yloxy)-acetic acid tert-butyl ester (1.32 g, 96%), which was used in the next step without further purification. MS cald. for C16H18ClFO4 328, obsd. 329 [(M+H)+].

1. extractionextracted with ethyl acetate (25 mL×3)
2. washwashed with water (25 mL×3)
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated in vacuo