反应详情

温度

0 °C

8-Phenyl-1,4-dioxaspiro[4.5]decane-8-carboxylic acid (3 g, 11.5 mmol) was initially introduced into anisole (30 ml). The suspension obtained was cooled to a temperature of 0° C. in an ice/sodium chloride bath and triethylamine (2.25 ml, 16 mmol) was added. A clear solutions was formed and was stirred at 0° C. for a further 15 min. Phosphoric acid diphenyl ester azide (2.5 ml, 11.5 mmol) was then added to the mixture in the course of 5 min. The reaction mixture was stirred at 0° C. for 20 min, allowed to come to RT in the course of a further 20 min and then heated in an oil bath at 100° C. (bath temperature) for 2 h. For working up, the anisole was distilled off under an oil pump vacuum. Purification by chromatography 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. customThe suspension obtained
2. customA clear solutions was formed
3. stirringThe reaction mixture was stirred at 0° C. for 20 min
4. customto come to RT in the course of a further 20 min
5. temperatureheated in an oil bath at 100° C. (bath temperature) for 2 h
6. distillationthe anisole was distilled off under an oil pump vacuum
7. customPurification by chromatography