反应详情

To a stirred solution of 2.0 g of 3-Chloro-6-(triphenylmethy)amino-α-(2-furanyl)ethynyl-α-(trifluoromethyl)benzyl alcohol (Example 9, Part B) in 20 mL of methanol was added 0.125 mL of 12 N aqueous hydrochloric acid, and the resulting solution was stirred at ambient temperature for 30 min. The reaction mixture was poured onto aqueous bicarbonate and extracted with ether. The ether layer was washed with brine, dried and evaporated. The residue was dissolved in methanol after cooling in ice for 1 h, the precipitated methyl trityl ether was filtered off. After evaporation of the filtrate, the residue was chromatographed over silica gel (elution with hexanes/ethyl acetate 3:1) affording after crystalization from hexane/ethyl acetate 280 mg of the title compound.

1. extractionextracted with ether
2. washThe ether layer was washed with brine
3. customdried
4. customevaporated
5. dissolutionThe residue was dissolved in methanol
6. temperatureafter cooling in ice for 1 h
7. filtrationthe precipitated methyl trityl ether was filtered off
8. customAfter evaporation of the filtrate
9. customthe residue was chromatographed over silica gel (elution with hexanes/ethyl acetate 3:1)
10. customaffording
11. customafter crystalization from hexane/ethyl acetate 280 mg of the title compound