Phosphine ligand compound and preparation method thereof, catalyst composition and application thereof and method for hydroformylation of vinyl acetate
A technology of vinyl acetate hydroformyl and vinyl acetate, which is applied in the field of phosphine ligand compounds and its preparation, can solve the problem of low selectivity of conversion rate 2-acetoxypropionaldehyde, and achieve the effect of improving selectivity
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[0048] According to a preferred embodiment of the present invention, the method for preparing the phosphine ligand comprises:
[0049] 1) Under nitrogen environment, add HO-B-OH to the reactor, then add PCl dropwise while stirring 3 , after the dropwise addition, the temperature was raised to 60-100°C, and the reaction was performed for 1-3h;
[0050] 2) Mix the compound shown in formula (6) with DMAP and solvent, and add dropwise to the reactor. After the dropwise addition, the temperature is raised to 40-60° C., and the reaction is carried out for 1-3h; the solvent is tetrahydrofuran; wherein, HO- B-OH and PCl 3 The molar ratio of the amount of the compound represented by the formula (6) is 1:(4-8):(0.5-2).
[0051] In the present invention, the progress of the reaction can be monitored by chromatography. After the reaction is completed, the obtained product can be post-treated by various post-treatment methods conventionally used in the art. The post-processing methods ...
preparation example 1
[0078] The preparation process of the compound shown in formula (2):
[0079]
[0080] 1) Evacuate the 50L reaction kettle, replace it with nitrogen three times, add 24.2mol ethylene glycol, start stirring, add 114.7mol phosphorus trichloride dropwise to the reaction kettle from the overhead tank, add 1h after finishing, heat up to 80°C, reflux The reaction was carried out for 2h. The reaction generates about 1800L of HCl gas, which is absorbed by a hydrochloric acid absorption tower. After the reaction was completed, the temperature was lowered to 40° C., and the phosphorus trichloride was evaporated under reduced pressure to the phosphorus trichloride high-level tank, recycled and reused, and the distillation loss was estimated to be 0.5 liters.
[0081] 2) 5L anhydrous tetrahydrofuran was added to the above-mentioned reaction kettle, and the premixed kettle was replaced with nitrogen, and 26.3mol of ethylene glycol and 12.3mol of acid binding agent DMAP (AR) were added ...
preparation example 2
[0086] The preparation process of the compound shown in formula (3):
[0087]
[0088] Carry out according to the method of preparation example 1, the difference is, the ethylene glycol two in step 2) is replaced with equimolar amount of The compound represented by formula (3) is obtained.
[0089] Overall yield: 82%.
[0090]NMR: 1H NMR (CDCl3 / TMS, 300MHz) δ (ppm): 1.34 (d, 3H, J=6.8Hz, CH3), 3.46-3.73 (m, 11H, CH2, CH).
[0091] Mass spectrum: [M+] 256.1334.
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