反应详情

温度

0 °C

11.1 g (1.3 eq) tert-butyl methyl(3-oxopropyl)carbamate were added to a solution of 11 g (1 eq) N,N-dimethyl-4-phenylpiperidin-4-amine dihydrochloride in 110 ml methanol at 0° C. and the reaction mixture was stirred for 15 min at 0° C. 6.2 g (3 eq) sodium cyanoboron hydride were then added in portions and the mixture was stirred for 30 min at room temperature. The reaction mixture obtained was adjusted to a pH of 5-6 with acetic acid and stirred for 12 h at room temperature. The reaction course was monitored by thin-layer chromatography (20% MeOH/CHCl3). As the conversion was still not complete, 2.4 g sodium cyanoboron hydride were added and the reaction mixture obtained was adjusted to pH 5-6 with acetic acid and stirred for 60 min at room temperature.

1. stirringthe mixture was stirred for 30 min at room temperature
2. customThe reaction mixture obtained
3. stirringstirred for 12 h at room temperature
4. customthe reaction mixture obtained
5. stirringstirred for 60 min at room temperature