反应详情

A solution of 1,2-bis(diphenylphosphino)-1′-diisopropylphosphino-4-[4-(1,3-dioxan-2-yl)-2-methylbut-2-yl]butylferrocene (1 g, 1.2 mmol) dissolved in 100 ml of THF is admixed with 15 ml of 2 N hydrochloric acid solution. After 2 hours with stirring at reflux, the reaction mixture is neutralized with saturated aqueous sodium hydrogencarbonate solution and extracted with 2×50 ml of CH2Cl2. The organic phase is dried over MgSO4 and concentrated on a rotary evaporator. The crude product obtained is purified by chromatography on silica gel (eluent AcOEt/heptane 1:4) to give 630 mg (ρ=67%) of 1,2-bis(diphenylphosphino)-1′-diisopropylphosphino-4-(4-oxo-2-methylbut-2-yl)ferrocene in the form of a red powder.

1. temperatureat reflux
2. extractionextracted with 2×50 ml of CH2Cl2
3. dry with materialThe organic phase is dried over MgSO4
4. concentrationconcentrated on a rotary evaporator
5. customThe crude product obtained
6. customis purified by chromatography on silica gel (eluent AcOEt/heptane 1:4)