反应详情

DDQ (1.1 eq) was added to a solution of (R)-N,N-diisopropyl-3-(2-hydroxy-5-hydroxymethylphenyl)-3-phenylpropanamine mandelate (prepared as described in WO 94/11337, Example 1) (2.46 g, 5 mmol), dichloromethane (20 mL) and phosphate buffer (pH 7) (0.1 mL). Thereafter, sodium hydroxide solution (20 mL, 1 M) and diethyl ether were added and the phases were separated. The water-phase was extracted twice with dichloromethane-diethyl ether (2:1). The organic phase was dried (MgSO4) and evaporated. The residue was crystallised from ethyl acetate-hexane to yield 1.35 g (80%).

1. customthe phases were separated
2. extractionThe water-phase was extracted twice with dichloromethane-diethyl ether (2:1)
3. dry with materialThe organic phase was dried (MgSO4)
4. customevaporated
5. customThe residue was crystallised from ethyl acetate-hexane
6. customto yield 1.35 g (80%)