反应详情

温度

0 °C

97 (0.07 g, 0.16 mmol) was dissolved in 10 mL of anhydrous CH2Cl2 under nitrogen at 0° C. Anhydrous AlCl3 (44 mg, 0.33 mmol) was added and the reaction mixture was stirred for 2 h at 0° C. Saturated NH4Cl (5 mL) was added and the organic phase was separated. The aqueous layer was extracted with CH2Cl2 (10 mL) and the combined organic phases were dried over Na2SO4, filtered, solvents evaporated under reduced pressure. The crude product was purified by column chromatography (30:70 EtOAc:Hexanes) to yield tan colored oil as product 24 (35 mg, 56% yield). Rf: 0.23 (60:40 Hex:EA).

1. customthe organic phase was separated
2. extractionThe aqueous layer was extracted with CH2Cl2 (10 mL)
3. dry with materialthe combined organic phases were dried over Na2SO4
4. filtrationfiltered
5. customsolvents evaporated under reduced pressure
6. customThe crude product was purified by column chromatography (30:70 EtOAc:Hexanes)