反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturecooling with ice
- stirringthe mixture was stirred at 5° to 10° C. for 2 hours
- stirringAfter stirring at room temperature for six hours
- customThe precipitate thereby formed
- filtrationwas filtered off