反应详情

温度

130 °C

5.5 g of trans-4-tert-butyloxycarbonylaminomethylcyclohexanecarboxylic acid are dissolved in 250 ml of dioxane and, after addition of 6.5 ml of triethylamine and 5.6 ml of diphenylphosphoryl azide, heated at 130° C. for 1.5 hours. Then 8.7 ml of benzyl alcohol are added and the mixture is heated to boiling for a further 48 hours. After cooling, the dioxane is distilled off in a rotary evaporator, the residue is taken up in ethyl acetate and, after washing with saturated sodium chloride solution and drying over magnesium sulphate, the solvent is distilled off in a rotary evaporator. The residue is triturated with petroleum ether/ether (5:1), filtered off with suction and dried.

1. temperaturethe mixture is heated
2. temperatureAfter cooling
3. distillationthe dioxane is distilled off in a rotary evaporator
4. washafter washing with saturated sodium chloride solution
5. dry with materialdrying over magnesium sulphate
6. distillationthe solvent is distilled off in a rotary evaporator
7. customThe residue is triturated with petroleum ether/ether (5:1)
8. filtrationfiltered off with suction
9. customdried