反应详情

温度

60 °C

N-{1-(1,2-Dihydronaphtho[2,1-b]furyl}-N-hydroxyurea. To a solution of N-{1-(1,2-dihydronaphtho[2,1-b]furyl}-N-hydroxyamine (698 mg, 3.5 mmol) in THF (10 mL) was added trimethylsilylisocyanate (0.94 mL, 7.0 mmol). The resulting solution was heated at 60° C. for 1 h, then allowed to cool and concentrated under reduced pressure. The residue was dissolved in EtOAc and washed successively with H2O and saturated aqueous NaCl. The solvent was removed in vacuo. The residue was triturated with Et2O and recrystallized from MeOH/CH2Cl2 /hexanes to provide the title compound (93 mg, 11%). m.p. 194.5°-195.5° C.

1. temperatureto cool
2. concentrationconcentrated under reduced pressure
3. dissolutionThe residue was dissolved in EtOAc
4. washwashed successively with H2O and saturated aqueous NaCl
5. customThe solvent was removed in vacuo
6. customThe residue was triturated with Et2O
7. customrecrystallized from MeOH/CH2Cl2 /hexanes