HRID231804

反应详情

EQUATION

反应方程式

HRID 231804 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 10 ml of benzene, 180 mg of 6-chloro-4-(1-pyrazolyl)pyrimidine, 175 ml of phenol, and 152 mg of 1,8-diazabicyclo-(5,4,0)-7-undecene (DBU) were dissolved, and refluxed for 7 hours. This reaction solution was washed with water, and an organic fraction was dried over anhydrous sodium sulfate. The resulting extract was distilled to give a residue, and the residue was purified by alumina gel column chromatography using a mixture of n-hexane and ethyl acetate (2:1) to yield 175 mg 6-phenoxy-4-(1-pyrazolyl)pyrimidine, recrystallized from n-hexane, to give an acicular crystal having a melting point of 92.5°-93.5° C.,

WORKUP

后处理

  1. temperaturerefluxed for 7 hours
  2. washThis reaction solution was washed with water
  3. dry with materialan organic fraction was dried over anhydrous sodium sulfate
  4. extractionThe resulting extract
  5. distillationwas distilled
  6. customto give a residue
  7. customthe residue was purified by alumina gel column chromatography
  8. additiona mixture of n-hexane and ethyl acetate (2:1)