HRID1108048

反应详情

EQUATION

反应方程式

HRID 1108048 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1-(2-benzyloxyethyl)thio-2-(2,4-difluorophenyl)-1,1-difluoro-3-(1H-1,2,4-triazol-1-yl)propan-2-ol (1.0 g, 2.2 mmol) in ethanol (20 ml), palladium black (20 mg, catalytic) was added, followed by stirring at room temperature and 1 atmospheric pressure in a hydrogen gas for 12 hours. After the completion of the reaction, an insoluble matter was filtered off. The solvent was then distilled off under reduced pressure. To the residue so obtained, water was added, followed by extraction with chloroform. The chloroform solution was washed with water, dried over magnesium sulfate and then distilled off under reduced pressure. To the residue, isopropyl ether was added for crystallization, whereby 2-(2,4-difluorphenyl)-1,1-difluoro-1-(2-hydroxyethyl)thio-3-(1H-1,2,4-triazol-1-yl)propan-2-ol (0.46 g, yield: 55.0%) was obtained as colorless crystals.

WORKUP

后处理

  1. customAfter the completion of the reaction
  2. filtrationan insoluble matter was filtered off
  3. distillationThe solvent was then distilled off under reduced pressure
  4. customTo the residue so obtained
  5. extractionfollowed by extraction with chloroform
  6. washThe chloroform solution was washed with water
  7. dry with materialdried over magnesium sulfate
  8. distillationdistilled off under reduced pressure
  9. additionTo the residue, isopropyl ether was added for crystallization