反应 #78158

反应方程式

1-chloro-4-(4-pyridylmethyl)phthalazine

p-toluidine

acetate

→

Title compound

1-(4-Methylanilino)-4-(4-pyridylmethyl)phthalazine

溶剂

potassium carbonate

反应条件

后处理

1. 1
   洗涤The organic phase washed with water
2. 2
   干燥dried over anhydrous sodium sulfate
3. 3
   其他is evaporated
4. 4
   其他the residue purified on silica gel by flash chromatography

实验过程

A mixture of 0.384 g (1.5 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine and 0.482 g (4.5 mmol) p-toluidine is stirred for 1.5 h at 90° C. under a nitrogen atmosphere. The reaction mixture is then distributed between 30 ml acetate and 20 ml of 20% aqueous potassium carbonate solution. The organic phase washed with water and dried over anhydrous sodium sulfate is evaporated and the residue purified on silica gel by flash chromatography using acetate/methanol mixtures (50:1 to 9:1). Title compound is obtained after crystallization of the product-containing fractions from acetonitrile and drying under HV; m.p. 152-153° C.; ESI-MS: (M+H)+=327.

来源