HRID919108

反应详情

EQUATION

反应方程式

HRID 919108 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-(Aminomethyl)cyclohexanecarboxylic acid (4.00 g, 25.44 mmol) was stirred in THF (100 mL) at 0° C. under a nitrogen atmosphere. LiAlH4 (2.90 g, 76.33 mmol) was then added and the reaction allowed to warm to RT and stir for 3 h. It was then cooled to 0° C. and quenched with H2O. Na2SO4 was then added and the mixture stirred for 10 minutes. It was then filtered through celite and the filtrate concentrated in vacuo to give the product as a colourless oil which solidified on standing to give the product as a white solid (3.72 g, 100%). 1H NMR (300 MHz, d6-DMSO) δ: 0.95 (4H, m), 1.22-1.47 (5H, m), 1.86 (4H, m), 2.55 (2H, d, J=6.6 Hz), 4.46 (2H, d, J=6.3 Hz).

WORKUP

后处理

  1. temperatureIt was then cooled to 0° C.
  2. customquenched with H2O
  3. additionNa2SO4 was then added
  4. stirringthe mixture stirred for 10 minutes
  5. filtrationIt was then filtered through celite
  6. concentrationthe filtrate concentrated in vacuo