反应详情

温度

80 °C

2.46 g (10 mmol) of 1,3-bis(hydroxymethyl)ferrocene and 4.72 g (40 mmol) of diisopropylphosphine were added to 40 ml of acetic acid. The resulting mixture was heated at 80° C. for 3.5 hours and extracted with benzene after cooling. The organic phase was then washed with water and then dried over Na2SO4. After evaporation an orange residue was chromatographed on an alumina column. Elution with an ether-light petroleum mixture yielded 3.92 g (88%) of the product. Selected NMR data (CDCl3, 22° C.) 1H: δ0.92 (m, 24H, CH3), 1.63 (m, 4H, CH(CH3)2), 2.49 (bs, 4H, CH2P), 3.92 (s, 5H, C5H5), 3.95 (bs, 2H, 4.5-H), 4.06 (bs, 1H, 2-H). 31P NMR (CDCl3, 22° C.): δ 10.97(s, 2P).

1. extractionextracted with benzene
2. temperatureafter cooling
3. washThe organic phase was then washed with water
4. dry with materialdried over Na2SO4
5. customAfter evaporation an orange residue
6. customwas chromatographed on an alumina column
7. washElution with an ether-light petroleum mixture