反应详情

The product from step 4 above (54 mg, 0.1 1 mmol) was dissolved in dry ether (20 mL), stirred at room temperature and treated with hydrogen chloride in ether (˜6 M; 5 mL). The resulting white suspension was stirred for 2 h, then quickly filtered off. The hydrochloride salt (hygroscopic), was dissolved in water and neutralized with sodium carbonate. The free base was extracted into dichloromethane. The organic layers were dried magnesium sulfat, filtered, and concentrated in vacuo to furnish 13 mg (29%) of the title product as a pale yellow oil. LS/MS purity 100%. 1H NMR (CDCl3) δ 1.8 (b, 1H); 2.45 (m, 4H); 2.95 (m, 4H); 3.45 (s, 2H); 3.55 (m, 4H); 3.7 (m, 4H); 4.35 (t, 2H); 4.7 (t, 2H); 6.85 (d, 1H); 6.95 (m, 2H); 7.25 (t, 1H); 7.55 (s, 1H); 7.75 (s, 1H).

1. stirringThe resulting white suspension was stirred for 2 h
2. filtrationquickly filtered off
3. dissolutionThe hydrochloride salt (hygroscopic), was dissolved in water and neutralized with sodium carbonate
4. extractionThe free base was extracted into dichloromethane
5. filtrationfiltered
6. concentrationconcentrated in vacuo