HRID1353193

反应详情

EQUATION

反应方程式

HRID 1353193 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2,7-dibromo-9-fluorenone (338 mg, 1.0 mmol) in dry THF (17 mL) under a nitrogen atmosphere were added copper(I) iodide (30 mg, 0.16 mmol) and dichlorobis(triphenylphosphine)palladium (II) (70 mg, 0.10 mmol), trans-3-methyl-2-penten-4-yn-1-ol (481 mg, 5.0 mmol) and dry isopropylamine (17 mL). After stirring at room temperature for 6 h, the reaction mixture was filtered and the filtrate evaporated to dryness. The product was purified by column chromatography on silica using dichloromethane/THF (10:1) as eluent to give 200 mg (71%) of (E)(E) 2,7-bis-(5-hydroxy-3-methyl-pent-3-en-1-ynyl)-fluoren-9-one.

WORKUP

后处理

  1. filtrationthe reaction mixture was filtered
  2. customthe filtrate evaporated to dryness
  3. customThe product was purified by column chromatography on silica