反应详情

To a solution of 87 mg of the resultant compound from Example 218 in 1 ml of DMF was added 0.028 ml of 3-aminomethylpyridine. After 18 hours, the solvent was removed in vacuo and the residue was dissolved in 1 ml of methanol and 0.05 ml of chlorotrimethylsilane was added. After 0.5 hour, the solvent was removed in vacuo, neutralized with sodium bicarbonate solution and extraction with ethyl acetate (2×25 ml). The organic solution was dried and concentrated. Purification by silica gel column chromotography provided 35 mg of desired product. 1H NMR (CD3OD): δ 1.60 (t, 2H), 2.60-2.80 (m, 4H), 3.70 (m, 1H), 4.00 (m, 1H), 4.10 (m, 1H), 4.25-4.35 (m, 4H), 7.10-7.25 (m, 10H), 7.35 (m, 2H), 7.60 (m, 2H), 8.40 (m, 4H). Mass spectrum: (M+H)+ =553.

1. customthe solvent was removed in vacuo
2. dissolutionthe residue was dissolved in 1 ml of methanol
3. addition0.05 ml of chlorotrimethylsilane was added
4. waitAfter 0.5 hour
5. customthe solvent was removed in vacuo
6. extractionneutralized with sodium bicarbonate solution and extraction with ethyl acetate (2×25 ml)
7. customThe organic solution was dried
8. concentrationconcentrated
9. customPurification by silica gel column chromotography