反应详情

温度

60 °C

A flask was charged with 9.7 g of magnesium and 200 ml of tetrahydrofuran, to which 43.2 g of 1,4-dibromobutane was added dropwise at 60° C. After the completion of dropwise addition, the contents were stirred for one hour at 60° C., and 22.6 g of methyl 2-hydroxy-3,3,3-trifluoro-2-trifluoromethylpropionate was added dropwise below 50° C. The mixture was stirred for one hour at room temperature, after which an ammonium chloride aqueous solution was added. This was followed by ordinary work-up and vacuum distillation, obtaining 22.4 g of the target compound (yield 89%).

1. additionwas added dropwise at 60° C
2. additionAfter the completion of dropwise addition
3. stirringThe mixture was stirred for one hour at room temperature
4. distillationThis was followed by ordinary work-up and vacuum distillation