HRID2111892

反应详情

EQUATION

反应方程式

HRID 2111892 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

N-(2-Methylpropyl)-N-[(quinolin-3-yl)methyl]piperidin-4-amine (0.74 g, 2.50 mmol) is dissolved in diethyl ether (35 ml) and methanol (6 ml). Fumaric acid (0.29 g, 2.50 mmol), in warm methanol (4 ml), is then added. Diethyl ether (100 ml) is added and the solution is heated. The solution is slowly cooled and then placed in the freezer. The solid is filtered and washed with diethyl ether to yield (0.79 g, 76%) of the title product: mass spectrum (ion spray): m/z=298.1 (M+1); 1H NMR (DMSO-d6): δ=8.84 (d, 1H), 8.16 (d, 1H), 7.98-7.91 (m, 2H), 7.71-7.68 (m, 1H), 7.58-7.54 (m, 1H), 6.42 (s, 2H), 3.75 (s, 2H), 3.25-3.22 (m, 2H), 2.76-2.70 (m, 3H), 2.21 (d, 2H), 1.83-1.59 (m, 6H), 0.76 (d, 6H).

WORKUP

后处理

  1. temperaturethe solution is heated
  2. temperatureThe solution is slowly cooled
  3. filtrationThe solid is filtered
  4. washwashed with diethyl ether