HRID259585

反应详情

EQUATION

反应方程式

HRID 259585 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7-Oxo-7-phenylheptanoylferrocene (1.94g; 5 mmole) was dissolved in 5% H2SO4 /acetic acid (40 ml; excess) at room temperature. The solution was stirred overnight and then poured into water (400 ml) and extracted with chloroform (3 × 200 ml). The organic layers were extracted with water, saturated aqueous sodium bicarbonate, and water, and dried (Na2SO4) to yield a brown oil. The crude occurrence product was suspended in hot petroleum ether (bp 40°-60° C.) and filtered. The filtrate was submitted to preparative thin layer chromatography on silica. The main yellow band was eluted with petroleum ether/ethyl acetate (10:1) and gave 670 mg (36.2%) of pure 3-benzoyl-2-ferrocenylcyclohexene mp 127°-129° C. EXAMPLE 8

WORKUP

后处理

  1. extractionextracted with chloroform (3 × 200 ml)
  2. extractionThe organic layers were extracted with water, saturated aqueous sodium bicarbonate, and water
  3. dry with materialdried (Na2SO4)
  4. customto yield a brown oil
  5. filtrationfiltered
  6. washThe main yellow band was eluted with petroleum ether/ethyl acetate (10:1)