Hydrochloric Acid → HCID 178446967、化合物

反応式

[C:1]1([P:7]([C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)[C-:8]2[CH:12]=[CH:11][C:10](CCCCC(C)(CCC3OCCCO3)C)=[C:9]2[P:28]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH:47]([P:50]([CH:56]([CH3:58])[CH3:57])[C-:51]1[CH:55]=[CH:54][CH:53]=[CH:52]1)([CH3:49])[CH3:48].[Fe+2:59].Cl.C(=O)([O-])O.[Na+].[CH2:66]1[CH2:70][O:69][CH2:68][CH2:67]1>>[C:1]1([P:7]([C:41]2[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=2)[C-:8]2[CH:12]=[C:11]([C:67]([CH3:68])([CH2:66][CH:70]=[O:69])[CH3:47])[CH:10]=[C:9]2[P:28]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH:56]([P:50]([CH:47]([CH3:49])[CH3:48])[C-:51]1[CH:55]=[CH:54][CH:53]=[CH:52]1)([CH3:58])[CH3:57].[Fe+2:59]

参加物

反応物 4

HCID 313Hydrochloric Acid

HCID 8028Tetrahydrofuran

HCID 516892Sodium Bicarbonate

HCID 178442532HCID 178442532、化合物

生成物 1

HCID 178446967HCID 178446967、化合物収率 67%

実験手順

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.