HRID491638

反应详情

EQUATION

反应方程式

HRID 491638 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

2-Methyl-4,5-dinitrophenol (Step A, 1.34 g, 6.77 mmol) and 4-chloro-pyridine-2-carboxylic acid methylamide (1.16 g, 6.77 mmol) were combined and heated at 160-180° C. (round bottom flask with condenser). The reaction was cooled to RT, the contents of the flask were dissolved in CH2Cl2 and the organic layer washed with 2 N NaOH, then water. The organic layer was dried with Na2SO4, filtered and evaporated. The mixture was purified by column chromatography using EtOAc/hexanes as the eluant. The title compound was obtained as a tan solid.

WORKUP

后处理

  1. temperatureThe reaction was cooled to RT
  2. washthe organic layer washed with 2 N NaOH
  3. dry with materialThe organic layer was dried with Na2SO4
  4. filtrationfiltered
  5. customevaporated
  6. customThe mixture was purified by column chromatography