反应详情

温度

80 °C

To a suspension of 1.5 g (4.5 mmol) of 4,5-bis(phenylmethoxy)-2-pyridinecarboxylic acid in 25 ml of t-butanol were added 1.5 g (5.4 mmol) of diphenylphosphoryl azide and 0.54 g (5.4 mmol) of triethylamine. The mixture was stirred at 80° C. for 17 hours. After cooling to room temperature, the crystals were filtered off, washed with ether and dried in vacuo. Yield: 1.3 g. Concentration of the mother liquor yielded another 0.3 g of product. Total yield: 1.6 g; melting point 163.3° C.

1. temperatureAfter cooling to room temperature
2. filtrationthe crystals were filtered off
3. washwashed with ether
4. customdried in vacuo