HRID851129

反应详情

EQUATION

反应方程式

HRID 851129 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

55 g (0.176 mol) of 1-(4-chlorophenoxy)-4-fluoro-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one (Example 1) were dissolved in 250 ml of methanol, and 3 g (0.08 mol) of sodium borohydride were added in portions. The reaction solution was subsequently stirred for 1 hour and then adjusted to a pH value of 3 with concentrated hydrochloric acid. After distilling off the solvent in vacuo, water was added to the residue and the mixture was extracted by shaking with methylene chloride. The combined organic phases were dried over sodium sulphate and concentrated in vacuo. The residue was crystallized with petroleum ether. 40 g (72% of theory) of 1-(4-chlorophenoxy)-4-fluoro-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-ol of melting point 103°-112° C. were obtained.

WORKUP

后处理

  1. distillationAfter distilling off the solvent in vacuo, water
  2. additionwas added to the residue
  3. extractionthe mixture was extracted
  4. stirringby shaking with methylene chloride
  5. dry with materialThe combined organic phases were dried over sodium sulphate
  6. concentrationconcentrated in vacuo
  7. customThe residue was crystallized with petroleum ether