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
- -60 °C
PROCEDURE
实验过程
In a nitrogen atmosphere, 1,2,3-trifluorobenzene was dissolved into THF, and cooled to −60° C. Then, butyllithium (1.56 M hexane solution) was added dropwise for 30 minutes, and stirred for 2 hours. Then, the THF solution containing iodine was added dropwise for 1 hour, and warmed to room temperature. After the reaction solution was poured into a sodium thiosulfate aqueous solution and stirred for a while, an organic layer was separated, and an aqueous layer was extracted with toluene. After the extract and the organic layer were mixed together, washed using water and a saturated saline solution in that order, and dried using anhydrous sodium sulfate, the solvent was evaporated under a reduced pressure to obtain 4-iodo-1,2,3-trifluorobenzene.
WORKUP
后处理
- additionwas added dropwise for 1 hour
- temperaturewarmed to room temperature
- stirringstirred for a while
- customan organic layer was separated
- extractionan aqueous layer was extracted with toluene
- extractionAfter the extract
- additionthe organic layer were mixed together
- washwashed
- customa saturated saline solution in that order, and dried
- customthe solvent was evaporated under a reduced pressure