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
- 50 °C
PROCEDURE
实验过程
To a solution of 2-(2,4-difluorophenyl)-1,1-difluoro-1-[(2-methoxyethyl)thio]-2,3-epoxypropane (13.0 g, 0.044 mol) in DMSO (100 ml), 1,2,4-triazole (7.6 g, 0.11 mol) and potassium carbonate (15.2 g, 0.11 mol) were added and the resulting mixture was stirred at room temperature for 12 hours and at an external temperature of 50° C. for one hour. After the completion of the reaction, the reaction mixture was diluted with ether and insoluble matter was filtered off. The ether solution was washed with water, dried over magnesium sulfate and distilled off under reduced pressure. The residue was recrystallized from isopropyl ether-ethyl acetate, whereby 2-(2,4-difluorophenyl)-1,1-difluoro-1-[(2-methoxyethyl)thio]-3-(1H-1,2,4-triazol-1-yl)-2-propanol (2.0 g, yield: 12.0%) was obtained as colorless crystals.
WORKUP
后处理
- customAfter the completion of the reaction
- filtrationwas filtered off
- washThe ether solution was washed with water
- dry with materialdried over magnesium sulfate
- distillationdistilled off under reduced pressure
- customThe residue was recrystallized from isopropyl ether-ethyl acetate