HRID903899

反应详情

EQUATION

反应方程式

HRID 903899 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

587 g (2 mols) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one were dissolved in 3 liters of methanol. A total of 80 g (2 mols) of sodium borohydride was added, in portions of 5 g each, to this solution at 0° to 10° C., while stirring and cooling with ice, and the mixture was stirred at 5° to 10° C. for 2 hours and then at room temperature for 12 hours. It was then cooled to 10° C. and 300 g (3 mols) of concentrated aqueous hydrochloric acid were added at 10° to 20° C. After stirring at room temperature for six hours, the resulting suspension was diluted with 3.8 liters of water which contained 400 g (4.8 mols) of sodium bicarbonate. The precipitate thereby formed was filtered off. 502 g (85% of theory) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-ol of melting point 112°-117° C. were obtained. ##STR12##

WORKUP

后处理

  1. temperaturecooling with ice
  2. stirringthe mixture was stirred at 5° to 10° C. for 2 hours
  3. stirringAfter stirring at room temperature for six hours
  4. customThe precipitate thereby formed
  5. filtrationwas filtered off