反应详情

A suspension of Pd/C (10%) (120 mg) and methyl 1-(4-nitrophenyl)cyclobutylcarbamate (A118) (404 mg, 1.61 mmol) in MeOH (17.0 mL) was vigorously stirred overnight under a hydrogen atmosphere. The resulting mixture was filtered through Celite then the filtrate concentrated in vacuo. The residue was purified using silica gel column chromatography (CombiFlash Rf, SiO2 cartridge, 0-75% EtOAc in cyclohexane) to give the title compound A119 (237 mg, 67%); 1H NMR (300 MHz, CDCl3); δ 7.21 (d, J=8.3 Hz, 2H), 6.63 (d, J=8.5 Hz, 2H), 5.57 (brs, 1H), 3.66 (s, 2H), 3.58 (s, 3H), 2.48 (m, 4H), 2.02 (m, 1H), 1.80 (m, 1H). LCMS-B: rt 2.35 min; m/z 221.2 [M+H]+.

1. filtrationThe resulting mixture was filtered through Celite
2. concentrationthe filtrate concentrated in vacuo
3. customThe residue was purified