反应详情

Platinum oxide (4.673 g, 20.58 mmol) was placed in a Parr bottle. Methanol (140 mL) was added under an atmosphere of nitrogen followed by (R)-(+)-3-methyl-2-(pyrazin-2-yl)butan-2-ol (17.1 g, 102.9 mmol). The reaction mixture was shaken in a PARR hydrogenator overnight with a hydrogen pressure of 60 psi. Lc/Ms after this time indicate that the reaction was complete. The suspension was filtered through a pad of Celite under a nitrogen atmosphere, rinsing with methanol. The crude mixture was concentrated in vacuo. The residue was re-dissolved in dichloromethane, dried over MgSO4, filtered and concentrated in vacuo to afford the title compound as viscous light yellow oil (16.6 g, 3:1 mixture of diastereoisomers, 93%); 1H NMR (CDCl3) 0.82-1.08 (9H, m), 1.81 (1H, m), 2.20-3.17 (10H, m); MS ES(+) 173.0 (M+1).

1. filtrationThe suspension was filtered through a pad of Celite under a nitrogen atmosphere
2. washrinsing with methanol
3. concentrationThe crude mixture was concentrated in vacuo
4. dissolutionThe residue was re-dissolved in dichloromethane
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo