反应详情

DIAD (9.62 g, 47.6 mmol) was added to a mixture of methyl 5-bromo-2-hydroxybenzoate (10 g, 43.3 mmol), 1,1-dimethylethyl (2-hydroxyethyl)carbamate (6.98 g, 43.3 mmol) and triphenylphosphine (12.47 g, 47.6 mmol) in THF (250 ml) and stirred at RT for 2.5 hr. Additional triphenylphosphine (2.5 g) was added followed by DIAD (4 ml) and the mixture left standing overnight. Evaporation and purification by flash chromatography eluting with 25% EtOAc/hexane gave the title compound as a yellow oil (8.92 g). MS (ES): C15H2081BrNO5 requires 375; found 276 [M+H−100]+.

1. waitthe mixture left
2. waitstanding overnight
3. customEvaporation and purification by flash chromatography
4. washeluting with 25% EtOAc/hexane