HRID1594095

反应详情

EQUATION

反应方程式

HRID 1594095 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The HCl salt of ethyl 2-chloro-acetimidate (3.90 g, 24.58 mmol) is added to a solution of N4-ethyl-6-trifluoromethyl-pyridine-3,4-diamine (1.44 g, 7.02 mmol) in EtOH (20 mL) and refluxed for 3 h. The reaction mixture is cooled to room temperature and concentrated under reduced pressure. The residue is diluted with CH2Cl2, washed with NaHCO3 solution, dried over Na2SO4, and concentrated to obtain 2-chloromethyl-1-ethyl-6-trifluoromethyl-1H-imidazo[4,5-c]pyridine. 1H NMR (300 MHz, CDCl3): δ 9.14 (s, 1H), 7.66 (s, 1H), 7.26 (s, 1H), 4.87 (s, 2H) 4.40 (t, J=7.5 Hz, 2H), 1.58 (t, J=7.5 Hz, 3H).

WORKUP

后处理

  1. temperaturerefluxed for 3 h
  2. concentrationconcentrated under reduced pressure
  3. additionThe residue is diluted with CH2Cl2
  4. washwashed with NaHCO3 solution
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated