HRID49861

反应详情

EQUATION

反应方程式

HRID 49861 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 1.28 g (5 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine and 1.64 ml (15 mmol) benzylamine is stirred for 4 min at 90° C. under a nitrogen atmosphere. The reaction mixture is then distributed between dichloromethane 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 and acetate/methanol (20:1). Title compound is obtained after crystallization of the product-containing fractions from acetonitrile and drying under HV (8 h, 80° C.); m.p. 137-138° C.; ESI-MS: (M+H)+=327.

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