反应详情

To a solution of the product of Step 2 (995 mg) in methanol (30 mL) under nitrogen was added Pd/C (169 mg). The flask was purged with hydrogen and stirred for 3 hours. Celite was added to the reaction mixture and it was filtered through a pad of Celite. The solvent was removed in vacuo. The resulting residue was purified by flash chromatography (ISCO, 0 to 10% methanol in dichloromethane) to afford the desired product (391 mg). 1H NMR (400 MHz, CDCl3): δ (ppm) 4.88 (br s, 2H), 2.58 (s, 1H), 1.44-1.41 (m, 2H), 1.41 (s, 6H), 1.06-1.03 (m, 2H).

1. customThe flask was purged with hydrogen
2. additionCelite was added to the reaction mixture and it
3. filtrationwas filtered through a pad of Celite
4. customThe solvent was removed in vacuo
5. customThe resulting residue was purified by flash chromatography (ISCO, 0 to 10% methanol in dichloromethane)