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
PROCEDURE
实验过程
11.8 g (0.04 mol) of 1-(6-chloropyridin-2-yl-oxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one (Example 1) were dissolved in 100 ml of methanol, and 1.8 g (0.04 mol) of sodium borohydride were added in portions at 20°-30° C., while stirring. After the exothermic reaction had ended, 5 ml of concentrated hydrochloric acid were added dropwise and the mixture was stirred at room temperature for 1 hour. Thereafter, 200 ml of water were added and the mixture was neutralised with sodium bicarbonate solution. The reaction mixture was extracted by shaking with ether and the organic phase was dried over sodium sulphate and concentrated. 5.3 g (54% of theory) of 1-(6-chloropyridin-2-yl-oxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butan-2-ol were obtained as a viscous oil in the form of a diastereomer mixture.
WORKUP
后处理
- customAfter the exothermic reaction
- stirringthe mixture was stirred at room temperature for 1 hour
- extractionThe reaction mixture was extracted
- stirringby shaking with ether
- dry with materialthe organic phase was dried over sodium sulphate
- concentrationconcentrated