反应详情

Compound (9) (1.000 g, 1,522 mmol) was dissolved in CH3OH (210 mL), followed by addition of 0.1N HCl (from concentrated HCl and methanol, 16.75 mL, 1.675 mmol) and 10% Pd-C. (0.6 g). The mixture was stirred under H2 (1 atm) at room temperature overnight. The catalyst was filtered and the solvent was removed. The residue was purified by Sephadex LH-20 column chromatography, eluting with 15% MeOH/toluene, to generate 560 mg (86%) of [A] as a colorless solid: NMR (CD3OD) δ 1.30-1.97 (m, 14 H) , 2.17 (s, 3 H), 2.60 (t, 4 H, J=6), 3.00 (t, 2 H, J=6), 3.70 (t, 6 H, J=6). Anal. (C17H35ClN4O6) C, H, N.

1. filtrationThe catalyst was filtered
2. customthe solvent was removed
3. customThe residue was purified by Sephadex
4. washcolumn chromatography, eluting with 15% MeOH/toluene