9,10-双(二乙基膦甲基)蒽

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Under an inert atmosphere, 3-bromobenzophenone (3.917 g, 15 mmol), and 9,10-bis(diethylphosphonomethyl)anthracene (2.942 g, 6.17 mmol) are dissolved in tetrahydrofuran (40 g). At room temperature, tetrahydrofuran (16.38 g) solution of tert-butoxy potassium (2.070 g, 18.45 mmol) is added dropwise for 5 minutes, and successively stirred for 3.5 hours. The reaction mixture is charged into water (200 ml) and neutralized with 5% sulfuric acid. After neutralization, a hydrophobic solvent is added and the organic layer is partitioned. The organic layer is washed with water and dried over anhydrous sodium sulfate. The solvent is distilled off under reduced pressure, and the resultant raw product is purified by silica gel chromatography or recrystallization to give a desired product. After neutralization, a hydrophobic solvent is added the organic layer is partitioned The organic layer is washed with water dried over anhydrous sodium sulfate The solvent is distilled off under reduced pressure the resultant raw product is purified by silica gel chromatography or recrystallization

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Under an inert atmosphere, 4-bromobenzophenone (3.917 g, 15 mmol), and 9,10-bis-(diethylphosphonomethyl)anthracene (2.942 g, 6.15 mmol) were dissolved in tetrahydrofuran (40 g). At room temperature, tetrahydrofuran (16.38 g) solution of tert-butoxy potassium (2.070 g, 18.45 mmol) was added dropwise for 5 minutes, and successively stirred for 3.5 hours. The reaction mixture was charged into water (100 ml) and neutralized with 5% sulfuric acid. After neutralization, the crystal was filtrated and the dissolved in tetrahydrofuran (300 ml). Then, the solvent was partly distilled off under reduced pressure, and cooled to deposit crystal. The crystal was filtrated and dried to give the desired product. (Yield: 1.10 g, 26%) After neutralization, the crystal was filtrated the dissolved in tetrahydrofuran (300 ml) Then, the solvent was partly distilled off under reduced pressure cooled The crystal was filtrated dried