HRID891964

反应详情

EQUATION

反应方程式

HRID 891964 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

4-Aminonicotinaldehyde (100 mg, 0.78 millimole (hereinafter “mmol”)), 2,6-dichlorophenylacetonitrile (217 mg, 1.2 mmol), 10% aqueous NaOH (0.101 mL, 0.25 mmol) and 700 uL of absolute ethanol are combined and heated at 65° C. for 24 hours (hereinafter “h”). The reaction mixture is cooled to ambient temperature and the solvents are evaporated under reduced pressure. The residue is diluted with 700 uL of DMSO filtered and purified with preparative reverse phase chromatography to afford the title compound as a yellow solid (191 mg, 84% yield). MS ES+ m/z=290.

WORKUP

后处理

  1. temperatureThe reaction mixture is cooled to ambient temperature
  2. customthe solvents are evaporated under reduced pressure
  3. additionThe residue is diluted with 700 uL of DMSO
  4. filtrationfiltered
  5. custompurified with preparative reverse phase chromatography