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1. Ommol of 0.2 ((1)) 8 was dissolved in 740 mmol of methanol,0.67 g of ligand G was added,And the mixture was stirred at room temperature for 2 hours.The catalyst solution was transferred to a 100 mL reaction vessel,Purge the reactor three times with nitrogen,Adding 50 mmol of ethylene oxide, carbon monoxide,So that the system pressure is 6. OMPa,Reaction at 65 C for 5 hours.The kettle body is fully cooled to 0 C,Slow pressure to atmospheric pressure,Purge the reactor three times with nitrogen,Sampling analysis,The results show:The conversion of ethylene oxide was 43%The selectivity of methyl 3-hydroxypropionate was 93%. |
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With pyridine; dicobalt octacarbonyl; at 60℃; under 37503.8 Torr; for 6h;Autoclave; Inert atmosphere; |
1, catalyst preparation1. Ommol of Co2 (C0) 8 was dissolved in 740 mmol of methanol, 2 mmol of pyridine was added to make the molar ratio of nitrogen to cobalt carbonyl 2: 1, and the mixture was stirred at room temperature for 2 hours to obtain a catalyst mixture. 2, Synthesis of methyl 3-hydroxypropionateThe resulting catalyst mixture was transferred to a 100 mL reaction vessel; the autoclave was purged with nitrogen three times,Carbon dioxide and 50 mmol of ethylene oxide, the system pressure of 5MPa; at 60 C for 6 hours. The reaction is over and the dad is coldBut to 0 C, slow pressure to atmospheric pressure, purging the reactor with nitrogen three times. Sampling analysis, the results show that: ethylene oxide conversionThe rate was 88% and the selectivity of methyl 3-hydroxypropionate was 82%. |
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With 1-benzyl-3-mesitylimidazol-3-ium bromide; In acetone; at 75℃; under 45004.5 Torr; for 5h;Inert atmosphere; |
In a 100-mL reaction tube, 5 mmol of ionic liquid H, 5 mmol of cuprous chloride, and 40 mL of acetone were added and reacted at room temperature for 12 hours. After the reaction was completed, the solvent acetone was removed under reduced pressure, and the catalyst H was obtained after vacuum drying.Add 1 mmol of Catalyst H to a 100 mL reactor. Purge the reactor three times with nitrogen and add 20 mmol of ethylene oxide.Acetone and 30 mL of methanol were passed through with carbon monoxide to make the pressure of the system 6.0 MPa and reacted at 75C for 5 hours.At the end of the reaction, the kettle body was sufficiently cooled to 0C and slowly depressurized to atmospheric pressure. The reactor was purged with nitrogen three times and sampled and analyzed. The experimental results are shown in Table 1. |
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With C19H21N2(1+)*CoCl2Br(1-); at 75℃; under 45004.5 Torr; for 5h;Inert atmosphere; |
1 mmol of Catalyst H was added to a 100 mL reactor, and the reactor was purged with nitrogen three times.20 mmol of ethylene oxide and 30 mL of methanol are added and carbon monoxide is introduced to make the system pressure 6.0 MPa.The reaction was carried out at 75 C for 5 hours. At the end of the reaction, the kettle body is cooled to 0C and slowly depressurized to atmospheric pressure.The reactor was purged with nitrogen three times and analyzed by sampling. The experimental results are shown in Table 1. |
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With C17H25N2(1+)*BrCl3Fe(1-); at 75℃; under 45004.5 Torr; for 5h;Catalytic behavior; |
1 mmol of catalyst E was added to a 100 mL reactor, and the reactor was purged with nitrogen three times. 20 mmol of ethylene oxide and 30 mL of methanol were added. Carbon monoxide was introduced to make the pressure of the system 6.0 MPa and reacted at 75 C. for 5 hours.At the end of the reaction, the kettle body was sufficiently cooled to 0C and slowly depressurized to atmospheric pressure. The reactor was purged with nitrogen three times and sampled and analyzed.The experimental results are shown in Table 1. |
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With pyridine; cobalt(III) phosphate; hydrogen; aluminium; at 0 - 60℃; under 67506.8 Torr; for 24h;Autoclave; |
In a 100 mL autoclave, 4.0 mmol of cobalt phosphate was added in sequence.6.0 mmol pyridine, 0.8 mmol aluminum powder, 40.0 mmol ethylene oxide, 750.0 mmol methanol.The kettle body was sufficiently cooled to 0 C, the air in the kettle was replaced with nitrogen three times, and a synthesis gas (H 2 /CO = 0.5:1) was introduced to bring the system pressure to 9 MPa, and the reaction was carried out at 60 C for 24 hours.After the reaction was completed, the autoclave was cooled to 0 C, and the pressure was slowly released to normal pressure. The reaction vessel was purged three times with nitrogen, and sampled and analyzed. The experimental results are shown in Table 1. |
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With C28H26ClN6Ru(2+)*2F6P(1-); In acetonitrile; at 50℃; under 30003 Torr; for 3h;Inert atmosphere; |
1 mmol of catalyst C was dissolved in 30 mL of methanol and 3 mL of acetonitrile.Transfer to a 100 mL reactor and purge with nitrogenThe reaction kettle was charged three times, 10 mmol of ethylene oxide was added, and carbon monoxide was introduced.The system pressure is 4.0 MPa, and the reaction is 3 hours at 50 C.Time. At the end of the reaction, the kettle body was cooled to 0 C.The pressure was slowly released to normal pressure, and the reaction vessel was purged three times with nitrogen, and sampled and analyzed.The experimental results are shown in Table 1. |
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With C4H6NS(1+)*Cl(1-)*CuCl; at 70℃; under 30003 Torr; for 3h;Inert atmosphere; |
1 mmol of catalyst A was added to a 100 mL reaction kettle, and the reaction kettle was purged three times with nitrogen.Add 10 mmol of ethylene oxide, 25 mL of methanol, and pass carbon monoxide.The system pressure was 4.0 MPa, and the reaction was carried out at 70 C for 3 hours.After the reaction is completed, the kettle body is sufficiently cooled to 0 C, and the pressure is slowly released to normal pressure.The reaction kettle was purged three times with nitrogen.Sampling analysis. The experimental results are shown in Table 1. |
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With C18H14CoN2O6; sodium methylate; at 80℃; under 91206.1 Torr; for 4h;Catalytic behavior; |
General procedure: Catalyst 1 of Structural Formula I was selected for investigation. The examples used methanol as a solvent and sodium methoxide as an auxiliary. In the case of methanol as a solvent, methanol is also one of the reactants therein, so the concentration of methanol is greatly excessive and can be measured without concentration. The reaction at a temperature change of 40, 60, 80, 100, 120, 140 0 was carried out at a holding pressure of 50 atm and a time of 4 h, and the results were recorded in Examples 1 to 6 of Table 1; the temperature was maintained at 80 C and the time was 4 h. The pressure changes were 5, 10, 30, 50, 70, 90, 100, and 120 atm, respectively, and the results were recorded in Examples 7 to 13 of Table 1. The temperature changes were maintained at a temperature of 80 C and a pressure of 30 atm, respectively. The results of the reactions of 2, 3, and 611 are shown in Tables 14 to 18 of Table 1, and the gas chromatogram of the product of Example 9 is shown in Fig. 1 . |
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General procedure: In a 100 mL reaction kettle, add 354 mg (6 mmol) of nano-cobalt catalyst, 466 mg (2 mmol) of alpha,alpha,alpha-terpyridine, and 30 mL of methanol. Purge the reactor three times with high purity nitrogen. Stir at 80C for 3 hours.The heating was stopped, the reaction kettle was cooled to room temperature, and the pressure was slowly released to normal pressure. A metering pump was injected with 2200 mg (50 mmol) of ethylene oxide. Carbon monoxide was added to make the system pressure 8 MPa, and the reaction was performed at 70C for 6 hours.The kettle body was fully cooled to -5C, and the pressure was slowly released to atmospheric pressure. The reaction kettle was purged with nitrogen three times and sampled for analysis. The results showed that the conversion rate of ethylene oxide was 75.9% and that of methyl 3-hydroxypropionate The selectivity is 92.8%. |
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