反应详情

To a solution of 2-methyl-3-(methylamino)-2-nitropropan-1-ol hydrochloride (5.4 g) in MeOH (32 ml) was added a slurry of Raney Nickel in H2O (1.5 ml). The vessel was pressurized with H2 (450 psi) and the suspension stirred for 48 h. The mixture was filtered through Celite and concentrated in vacuo to give 7.4 g of a crude liquid, which was used directly in the next step without purification. 1H NMR (400 MHz, CDCl3) δ 1.01 (s, 3H), 2.26 (s, 3H), 2.99 (s, 2H), 3.41-3.44 (d, J=11.6 Hz, 1H), 3.48-3.51 (d, J=11.6 Hz, 1H). LRMS (ESI/APCI): 145 [M+H]+.

1. filtrationThe mixture was filtered through Celite
2. concentrationconcentrated in vacuo