HRID1765001

反应详情

EQUATION

反应方程式

HRID 1765001 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionwas added dropwise for 30 minutes
  2. stirringstirred for a while
  3. customan organic layer was separated
  4. extractionan aqueous layer was extracted with toluene
  5. extractionAfter the extract
  6. additionthe organic layer were mixed together
  7. washwashed
  8. customa saturated saline solution in that order, and dried
  9. customthe solvent was evaporated under a reduced pressure
  10. customThe residue was purified by column chromatography (silica gel, hexane)