反应详情

A mixture of 4-benzyloxybenzaldehyde (20 g, 94.23 mmol), N-cyclopentylhydroxylamine (14.3 g, 141.34 mmol), molecular sieves (60 g, 4A) and silica gel (15 g) in chloroform (300 mL) was stirred at room temperature under argon atmosphere for 48 hrs and then was refluxed for an additional 3 hrs. The mixture was filtered and rotary evaporated to give crystals which were recrystallized from hexanes and EtOAc to provide the title compound as white crystals, 23.7 g, 85.1% yield), m.p. 115.1° C. (Rf=0.35 on a silica gel plate using hexanes:EtOAc, 1:1, v:v, as an eluant).

1. temperaturewas refluxed for an additional 3 hrs
2. filtrationThe mixture was filtered
3. customrotary evaporated
4. customto give crystals which
5. customwere recrystallized from hexanes and EtOAc