向3.15 g(20 mmol)4-羟基-6,6-二甲基-5,6-二氢吡啶-2(1H)-硫酮在200 ml EtOH中的溶液中加入15克新鲜制得的雷尼镍,然后在在50℃,45psi的氢气下搅拌48小时. 过滤后,蒸发溶剂. 将残余物溶解在CHCl3中,过滤,用H 2 O洗涤并干燥. 除去溶剂,并在真空中蒸馏出2,2-二甲基哌啶-4-醇.馏出物重结晶.产量:2.24g(87%).m.p. (EtOH/H 2 O) = 78 C; bp:66 ℃/0.2 mbar; IR (KBr) 3254, 2930, 2843, 1452, 1364,1260, 1146, 1117, 1072 cm -1 ; 1 H NMR (400 MHz, CDCl 3)d 1.10 (s, 3H, CH3ax), 1.13 (t, J =12.3 Hz, 1H, 3-Hax),1.16 (s, 3H, CH3eq), 1.23 (dddd, J = 13.0, 12.3, 10.0,4.7 Hz, 1H, 5-Hax), 1.84 (ddd, J = 12.3, 4.3, 2.0 Hz, 1H,3-Heq), 1.90e1.98 (m, 1H, 5-Heq), 2.81 (ddd, J =13.4,12.3, 2.9 Hz, 1H, 6-Hax), 2.96 (ddd, J = 13.4, 4.7, 2.7 Hz,1H, 6-Heq), 3.80-3.88 (m, 1H, 4-Hax) ppm; 13 C NMR(100 MHz, CDCl 3) 24.47 (CH3ax), 32.64 (CH3eq), 36.53(C-5), 40.01 (C-6), 47.70 (C-3), 51.17 (C-2), 66.22 (C-4) ppm;Anal. C7H15NO (C, H, N).
产品链接: CAS No. 937681-12-4››联系我们可以获取更多内容.
如有产品相关项目调研或推广服务, 请致函联系我们