反应详情

Compound 133 (1.25 g 2 mmole) was dissolved in dry CH2Cl2 (20 ml) and this solution was cooled in an acetone-dry ice bath. A 1 M solution of BCl3 in CH2Cl2 (10 ml) was added and the mixture was stirred at -70° for 4.5 hr. At this point TLC showed no starting material. CH3OH (10 ml) was added and the solution was made neutral with NH4OH. The solution was evaporated in vacuo to dryness. H2O (20 ml) was added and the solution was extracted with EtOAc. The EtOAc layer was washed with H2O, dried (Na2SO4) and evaporated in vacuo to obtain a syrup. This syrup was subjected to flash column chromatography on silica gel (Kieselgel 60, 230-400 mesh) with CH2Cl--MeOH (20:1) as eluent solvent to give 134. Yield 0.551 g, 77.9%.

1. temperaturethis solution was cooled in an acetone-dry ice bath
2. customThe solution was evaporated in vacuo to dryness
3. additionH2O (20 ml) was added
4. extractionthe solution was extracted with EtOAc
5. washThe EtOAc layer was washed with H2O
6. dry with materialdried (Na2SO4)
7. customevaporated in vacuo
8. customto obtain a syrup