HRID1160981

反应详情

EQUATION

反应方程式

HRID 1160981 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

15.2 g (45 mmol) of 2,7-dibromo-9-fluorenone was put in a 100 mL three-necked flask, and nitrogen substitution was conducted. 40 mL of diethyl ether was added. The Grignard reagent above was transferred into a dropping funnel by a cannula so as not to expose it to the atmosphere, and was added dropwise into the mixture. The mixture was refluxed at 50° C. After the reaction, the solution was washed with water. Then the aqueous layer was extracted with ethyl acetate and combined with the organic layer. The layers were washed with a saturated saline solution, then dried with magnesium sulfate. Filtration and concentration were carried out, and 22 g of 9-(biphenyl-2-yl)-2,7-dibromo-9-fluorenol was obtained as a white solid, in a yield of 90%.

WORKUP

后处理

  1. additionwas added dropwise into the mixture
  2. customAfter the reaction
  3. washthe solution was washed with water
  4. extractionThen the aqueous layer was extracted with ethyl acetate
  5. washThe layers were washed with a saturated saline solution
  6. dry with materialdried with magnesium sulfate
  7. filtrationFiltration and concentration