[Li]CCCC.Br[C-:7]1[CH:11]=[CH:10][CH:9]=[CH:8]1.[C-:12]1([Br:17])[CH:16]=[CH:15][CH:14]=[CH:13]1.[Fe+2:18].[Cl-].[CH:20]1([PH:26][CH:27]2[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]2)[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1.O>C1COCC1.CCCCCC>[CH:27]1([P:26]([CH:20]2[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25]2)[C-:7]2[CH:11]=[CH:10][CH:9]=[CH:8]2)[CH2:28][CH2:29][CH2:30][CH2:31][CH2:32]1.[Br:17][C-:12]1[CH:16]=[CH:15][CH:14]=[CH:13]1.[Fe+2:18]
120 ml (0.3 mol) of n-BuLi (2.5 M in hexane) are added dropwise to a solution of 103 g (0.3 mol) of 1,1′-dibromoferrocene in 300 ml of THF at a temperature of <−30° C. The mixture is stirred at this temperature for a further 1.5 hours. It is then cooled to −50° C. and 66.2 ml (0.3 mol) of dicyclohexylphosphine chloride are added dropwise at such a rate that the temperature does not exceed −45° C. After stirring the mixture for a further 10 minutes, the temperature is allowed to rise to room temperature and the mixture is stirred for another one hour. After addition of 150 ml of water, the reaction mixture is shaken with hexane. The organic phases are dried over sodium sulphate and the solvent is distilled off under reduced pressure on a rotary evaporator. The residue is crystallized in ethanol. The product A2 is obtained in a yield of 84% (yellow solid). 1H NMR (300 MHz, C6D6): δ 1.20-2.11 (m, 22H), 3.97 (m, 2H), 4.23 (m, 2H), 4.26 (m, 2H), 4.41 (m, 2H). 31P NMR (121.5 MHz, C6D6): δ −8.3 (s).
読み込み中…
