Bisphosphite ligands for hydroformylation catalyzed by transition metals
A bisphosphite, phosphite technology, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, organic chemistry and other directions, can solve problems such as only regioselectivity, and achieve high Effects of stability and low isomerization activity
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Embodiment 1
[0114] Example 1: Synthesis of 1-chloro-3,3,4,4-tetraphenylphosphorane (phos pholan) (C-1)
[0115]
[0116] Under stirring at -40°C, a 0.768M solution of phosphorus trichloride (Aldrich, 99%) in tetrahydrofuran (10.7mL; 8.22mmol) was added dropwise to 1.878g (5.12mmol) of tetraphenylethylene glycol (Benzo pinakol). ) (Acros, 98%) in a suspension of 30 mL of tetrahydrofuran (Sigma-Aldrich, 99.9%), followed by dropwise addition of 1.56 g (15.4 mmol) of triethylamine (Aldrich, pa) in 4 mL of tetrahydrofuran, the result A large amount of colorless precipitate is formed. The mixture was allowed to warm to room temperature and stirred for another 5 h. The reaction mixture was filtered through G4 porous glass, and the filtrate was dried at 40° C. and 20 mbar for 1.5 h. The viscous residue was absorbed in toluene (15 mL). The solution was filtered through G4 porous glass, and the filtrate was evaporated at 20 mbar, followed by a bath temperature of 10 at 40℃ -1 Dry for 2h under mbar....
Embodiment 2
[0122] Example 2: Synthesis of A-1
[0123]
[0124] Prepare A1 according to the method described in EP 1 209 164, starting material 2,2′-bis(6-tert-butyl-1-hydroxy-4-methoxyphenyl) (according to FR Hewgill and DGHewitt in Journal of the Chemical Prepared by the method described in Society C, 1967, 8, 726-730).
[0125] Synthesis of B-2
[0126]
[0127] B-2 was prepared from A-1 according to the method described in EP 1 209 164 (Example 2).
[0128] Synthesis of D-2
[0129]
[0130] A solution of n-butyllithium (2.014 mmol) in hexane (4 mL) was added dropwise with stirring to a solution of B-2 (1.5 g; 2.014 mmol) in THF (8 mL) previously cooled to -20°C. 20min after the addition is complete, let the mixture warm to room temperature and slowly add 2-chloro-4,4',5,5'-tetraphenyl-1,3,2-dioxaphosphorane (C-1)( 0.868 g; 2.014 mmol) in THF (8 mL). The mixture was stirred at room temperature for 4 h, then the solvent was driven off at 40 mbar, and the residue was heated at -1 Drying is c...
Embodiment 3
[0132] Example 3: Synthesis of D-3
[0133]
[0134] Triethylamine (0.992g; 9.81mmol) was first added to the suspension of racemic-1,1'-bis(2-naphthol) (0.891g, 3.113mmol, Aldrich, 99%) in 18mL of toluene at room temperature Then, a solution of C-1 (2.951 g; 6.85 mmol) in 26 mL of toluene was added with stirring at 0°C. The mixture was stirred at 0°C for another 45 min, followed by stirring at 80°C for 16 h. The product obtained is filtered, the solvent is removed at 20 mbar, the residue is stirred with 10 mL of toluene and filtered again. The filtrate was evaporated and the highly viscous residue was obtained at 55°C and 10 -1 Dry for 2 h at mbar, then recrystallize from acetonitrile. Yield: 2.684 g (2.496 mmol; 80% of theoretical value). Analysis (calculated value C 72 H 52 O 6 P 2 =1075.14g / Mol) C 79.63(80.43); H 4.69(4.87); P 6.03(5.76)%. 31 P-NMR(CD 2 Cl 2 )δ140.5ppm.
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