反应详情

温度

80 °C

A solution of 80 g of 1-(methoxycarbonyl)cyclopropane carboxylic acid and 78 ml of triethylamine in 550 ml of toluene, to which 152 g of diphenylphosphoryl azide are added, is heated at 80° C. After the evolution of gas has ceased, the temperature is brought to 50° C. and 61 g of tert-butanol are added. After reacting for 7 hours at 80° C., the mixture is concentrated. The residue is taken up in ether, washed with saturated Na2CO3 solution, then with 1N hydrochloric acid solution and then with NaHCO3 solution. After drying and evaporation of the organic phase, the residue is taken up in 300 ml of cyclohexane and then concentrated to dryness. The residue obtained is triturated in pentane, filtered and then dried, allowing the expected product to be isolated.

1. customis brought to 50° C.
2. concentrationthe mixture is concentrated
3. washwashed with saturated Na2CO3 solution
4. customAfter drying
5. customevaporation of the organic phase
6. concentrationconcentrated to dryness
7. customThe residue obtained
8. customis triturated in pentane
9. filtrationfiltered
10. customdried
11. customto be isolated