反应详情

Raney nickel (W-2 grade, 7.60 g) and concentrated NH4OH (10 mL) were successively added to 38 (5.06 g, 14.6 mmol) in CH3OH (30 mL) and THF (30 mL) in a 200 mL Parr bottle, and a slow stream of NH3 was bubbled through the mixture for 30 minutes at 0° C. After hydrogenation in a Parr bottle was carried out at 50-55 psi for 8 hours, the suspension was filtered through Celite, and the solvents were removed in vacuo to give 4.70 g (91%) of 41 as an oil: NMR δ 1.14-1.24 (m, 10 H), 2.25 (s, 3 H), 2.6 (s, 6 H), 3.05-3.25 (m, 8 H), 3.45 (s, 4 H), 6.9 (s, 2 H).

1. customa slow stream of NH3 was bubbled through the mixture for 30 minutes at 0° C
2. filtrationthe suspension was filtered through Celite
3. customthe solvents were removed in vacuo