HRID889103

反应详情

EQUATION

反应方程式

HRID 889103 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

(2-Chloro-quinazolin-4-yl)-phenyl amine (250 mg, 0.98 mmol) was dissolved in acetonitrile (4 mL) and 3,5-dimethylpyrazole (140 mg, 1.47 mmol) was added. The mixture was heated in a sealed tube at 130° C. for 12 hours. The mixture was concentrated and the residue basified with sodium hydrogencarbonate, extracted with chloroform dried over anhydrous sodium sulfate filtrated and evaporated. The crude product was purified by column chromatography (ethylacetate/hexane) to give [2-(3,5-dimethyl-pyrazol-1-yl)-quinazolin-4-yl]-phenyl-amine (150 mg, 49%). Mp. 262.4-265.3° C.

WORKUP

后处理

  1. concentrationThe mixture was concentrated
  2. extractionextracted with chloroform
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltrated
  5. customevaporated
  6. customThe crude product was purified by column chromatography (ethylacetate/hexane)