反应详情

温度

0 °C

Methyl 2-(2-bromo-5-phenylthiophen-3-yl)-2-hydroxyacetate (11h) (75 mg, 0.23 mmol) was dissolved in tert-butyl acetate (8.6 mL) at 0° C. and 70% perchloric acid (1.1 mL) was rapidly added. The mixture was stirred at 0° C. for 30 minutes then poured in a saturated solution of potassium carbonate. Layers were separated. The aqueous layer was extracted with ethyl acetate (2×15 mL). The organic layers were washed with brine (8 mL), dried over sodium sulfate and concentrated in vacuo to provide the desired product (11i) (77 mg, 0.20 mmol, 87%) which was used without further purification.

1. customLayers were separated
2. extractionThe aqueous layer was extracted with ethyl acetate (2×15 mL)
3. washThe organic layers were washed with brine (8 mL)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo