反应详情

To a solution of 1.0 g of 3-tert-butoxycarbonylamino-4-hydroxybutyronitrile in 15 ml of tetrahydrofuran are added 0.85 g of 5-chloro-3-hydroxy-1,2-benzoisoxazole, 1.71 g of triphenylphosphine and 1.14 g of diethyl azodicarboxylate with ice-cooling, and they are subjected to reaction at room temperature for 24 hours. Thereafter, the solvent is removed by distillation under reduced pressure. The residue obtained is purified by a column chromatography [eluant:n-hexane:ethyl acetate=5:1], to obtain 1.29 g of 3-(2-tert-butoxycarbonylamino-3-cyanopropoxy)-5-chloro-1,2-benzoisoxazole having a melting point of 147.2°-147.9° C.

1. temperaturecooling
2. customthey are subjected to reaction at room temperature for 24 hours
3. customThereafter, the solvent is removed by distillation under reduced pressure
4. customThe residue obtained
5. customis purified by a column chromatography [eluant:n-hexane:ethyl acetate=5:1]