反应详情

温度

0 °C

8-phenyl-1,4-dioxaspiro[4.5]decane-8-carboxylic acid (3 g, 11.5 mmole) was added to anisole (30 ml). The resultant suspension was cooled to a temperature of 0° C. in an ice-salt bath and triethylamine (2.25 ml, 16 mmole) was added. A clear solution was formed, which was stirred for a further 15 minutes at 0° C. Phosphoric acid diphenyl ester azide (2.5 ml, 11.5 mmole) was then added to the mixture within 5 minutes. The reaction mixture was stirred for 20 minutes at 0° C., left to cool to RT within a further 20 minutes, and was then heated in an oil bath for 2 hours at 100° C. (bath temperature). The reaction mixture was worked up by distilling off the anisole under an oil pump vacuum. The chromatographic purification was carried out on silica gel with toluene. The desired product was obtained as a crystalline solid with a melting point of 38°-41° C. in a yield of 2.7 g (91%).

1. customA clear solution was formed
2. stirringThe reaction mixture was stirred for 20 minutes at 0° C.
3. waitleft
4. temperatureto cool to RT within a further 20 minutes
5. temperaturewas then heated in an oil bath for 2 hours at 100° C. (bath temperature)
6. distillationby distilling off the anisole under an oil pump vacuum
7. customThe chromatographic purification