反应详情

A mixture of hydroxyl-[4-(4-isopropyl-piperazine-1-carbonyl)-phenyl]-methanesulfonic acid sodium salt (54.6 g, 0.150 mol), piperidine (28.0 g, 0.330 mol), and Montmorillonite-K10 (10.9 g, 20% by wt. relative to starting material) in dichloroethane (820 mL) was stirred at room temperature for 16 h. NaBH(OAc)3 (44.5 g, 210.0 mmol) was added in portions over 1 h, and the resulting suspension was stirred at room temperature for 5 h. Diatomaceous earth (5.4 g) was added and the suspension was stirred for an additional 30 min. The reaction mixture was filtered through a pad of diatomaceous earth, rinsing with dichloroethane (2×100 mL). The filtrate was washed with 1 N NaOH (2×200 mL). The aqueous layers were combined and back-extracted with dichloroethane (2×100 mL). The organic layers were combined, dried (Na2SO4), and concentrated to yield the title compound as its corresponding free base, as a pale yellow oil.

1. stirringthe resulting suspension was stirred at room temperature for 5 h
2. additionDiatomaceous earth (5.4 g) was added
3. stirringthe suspension was stirred for an additional 30 min
4. filtrationThe reaction mixture was filtered through a pad of diatomaceous earth
5. washrinsing with dichloroethane (2×100 mL)
6. washThe filtrate was washed with 1 N NaOH (2×200 mL)
7. extractionback-extracted with dichloroethane (2×100 mL)
8. dry with materialdried (Na2SO4)
9. concentrationconcentrated