反应详情

Compound 132 (6.13 g, 16.6 mmol), 4-nitrobenzoic acid (4.17 g, 25 mmol) and PPh3 (6.55 g, 25 mmol) was dissolved in THF (130 ml). The solution was cooled to ˜0° and diisopropyl azidocarboxylate (5.1 g, 25 mmol) was added slowly. The cooling was then removed and the mixture was left over-night at ambient condition. Aqueous sodium hydrogen carbonate (60 ml) was added and the mixture was extracted with dichloromethane. Purification by flash chromatography (pentane-ether, 2:1→pentane-ether, 1:2→2% methanol in ether) gave pure title compound (6.2 g, 72%).

1. temperatureThe solution was cooled to ˜0°
2. customThe cooling was then removed
3. waitthe mixture was left over-night at ambient condition
4. additionAqueous sodium hydrogen carbonate (60 ml) was added
5. extractionthe mixture was extracted with dichloromethane
6. customPurification by flash chromatography (pentane-ether, 2:1→pentane-ether, 1:2→2% methanol in ether)