反应详情

The intermediate obtained in Step B (349 mg, 0.40 mmol) was dissolved in 5 mL of methanol and hydrogenated at room temperature and one atmosphere over 70 mg of 20% Pd(OH)2 /C for 16 hours. The reaction mixture was filtered through Celite and solvent removed under vacuum. The crude product was purified by flash chromatography on silica, eluting with 10% methanol/ethyl acetate to afford 168 mg (0.28 mmol, 71%) of product. 1H NMR (200 MHz, CD3OD): 1.41 (s,9H), 1.72 (m,2H), 2.0-2.6 (m,6H), 3.24 (t,7 Hz,2H), 4.32 (m,1H), 4.85 (d,14 Hz,1H), 5.20 (d,14 Hz,1H), 6.9-7.7 (m,12H).

1. filtrationThe reaction mixture was filtered through Celite and solvent
2. customremoved under vacuum
3. customThe crude product was purified by flash chromatography on silica
4. washeluting with 10% methanol/ethyl acetate