反应详情

温度

95 °C

To a mixture of compound 51, prepared according to Scheme 6, (0.25 g, 0.625 mmole) in toluene (5 mL), was added diphenylphosphorylazide (0.192 g, 0.70 mmole) and triethyl amine (0.1 mL, 0.7 mmole). After stirring the mixture under argon at 95° C. for two hours an excess of anhydrous ethanol (2 mL) and triethylamine (0.1 mL) were added and the solution was stirred at 95° C. for an additional 5 hours. After cooling to room temperature the reaction mixture was partitioned between water and diethyl ether. The ether was washed with water, dried over magnesium sulfate and removed in vacuo to give the product (compound 88) as a tan foam (300 mg, 99% yield).

1. customprepared
2. additionwere added
3. temperatureAfter cooling to room temperature the reaction mixture
4. customwas partitioned between water and diethyl ether
5. washThe ether was washed with water
6. dry with materialdried over magnesium sulfate
7. customremoved in vacuo