HRID558583

反应详情

EQUATION

反应方程式

HRID 558583 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 3-trifluoromethyl-5-(4-trifluoromethyl-phenyl)-pyridin-2-ylamine (12.77 g, 42 mmol) and NaHCO3 (5.96 g, 71 mmol) in EtOH (300 mL) was added chloracetaldehyde solution 55% in water (22 mL, 188 mmol), then refluxed overnight. The reaction mixture was concentrated and purified by column chromatography (CH2Cl2/Et2O 1:1) to give the product as a white crystalline solid (9.6 g, 69%). MS (ISP) 331.1 [(M+H)+].

WORKUP

后处理

  1. temperaturerefluxed overnight
  2. concentrationThe reaction mixture was concentrated
  3. custompurified by column chromatography (CH2Cl2/Et2O 1:1)