HRID1765001
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
Sodium hydride (60% in oil) was suspended in DMF under nitrogen replacement. Then, the THF solution containing 1-(3-hydroxy-1-hexyl)-2,3,4-trifluorobenzene was added dropwise for 30 minutes, and stirred for 3 hours at 50° C. After toluene was added 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. The residue was purified by column chromatography (silica gel, hexane) to obtain 7,8-difluoro-2-propylchroman.
WORKUP
后处理
- additionwas added dropwise for 30 minutes
- 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
- customThe residue was purified by column chromatography (silica gel, hexane)