HRID64645

反应详情

EQUATION

反应方程式

HRID 64645 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5.1 g 2-(4-ethynylphenyl)-3-methyl-1-(1H-1,2,4-triazole-1-yl)butan-2-ol in 100 ml abs. CH3OH are simultaneously added, with stirring at 20°-25°, 2.6 g iodine and 10 ml 30% NaOH solution. The reaction mixture is maintained at room temperature for 24 hours, with stirring, then poured into 500 ml H2O and extracted with CH2Cl2. The organic phase is washed, dried and evaporated. The residue is stirred in hexane fraction and kept over 16 hours at rest. The precipitate is sucked off and dried to give the title compound m.p. 122° as colourless crystals.

WORKUP

后处理

  1. stirringwith stirring
  2. extractionextracted with CH2Cl2
  3. washThe organic phase is washed
  4. customdried
  5. customevaporated
  6. stirringThe residue is stirred in hexane fraction
  7. customdried