HRID49865

反应详情

EQUATION

反应方程式

HRID 49865 的结构方程式

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 0.511 g (2 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine and 0.565 g (6 mmol) 3-aminopyridine is heated for 3 h at 90° C. The residue is then distributed between acetate and 20% aqueous potassium carbonate solution. The organic phase dried over anhydrous sodium sulfate is evaporated and the residue purified on silica gel by flash chromatography using acetate/methanol mixtures (49:1 to 4:1). Title compound is obtained after crystallization of the product-containing fractions from acetonitrile and drying under HV (6 h, 80° C.); m.p. 137-139° C.; ESI-MS: (M+H)+=314.

WORKUP

后处理

  1. dry with materialThe organic phase dried over anhydrous sodium sulfate
  2. customis evaporated
  3. customthe residue purified on silica gel by flash chromatography