| 98% |
With phosphorus modified SO4(2-)/TiO2; In cyclohexane; for 2h;Dean-Stark; Reflux; |
General procedure: Aldehyde or ketone (20 mmol), diol (24 mmol), 5 mL cyclohexane, and the catalyst (20 mg) were mixed together in a three necked round bottomed flask equipped with a magnetic stirrer and a thermometer, and a Dean-Stark apparatus which was constituted with manifold and condenser to remove the water continuously from the reaction mixture. The reaction was refluxed for 2h to complete the reaction. |
| 93.2% |
With sulfonic acid-functionalized mesoporous chromium (III)terephthalate; In cyclohexane; at 80℃; for 4h;Catalytic behavior; |
General procedure: The liquid-phase acetalization was conducted in a three-necked round-bottom flask connected with a reflux condenser and a thermometer. The typical procedures for acetalization were as follows: benzaldehyde (7.42 g, 70 mmol), glycol (7.81 g, 126 mmol), catalyst (0.12 g), and cyclohexane (8 mL, as a water-carrying agent) were charged successively into the flask and heated at 80 C under stirring. The reaction mixtures were sampled periodically and analyzed using a GC (GC-2014) equipped with an FID detector and a capillary column (DB-5, 30 m × 0.45 mm × 0.42 mum). After the reaction, the catalyst was separated from the reaction medium by centrifugation, washed with acetone (3-4 times) and treated at 150 C for 180 min for activation, and then reused in the next run. |
| 87.22% |
for 2h;Reflux; |
Epoxidation reaction: 500 g of propionitrile and 12.5 g of phosphotungstic acid catalyst were placed in a 1 L autoclave, filled with 61.8 g of propylene (1.47 mol), the reaction was vigorously stirred at 70 C for 4 h, and the temperature was lowered, the pressure was released, and the sample was analyzed. The conversion rate of hydrogen peroxide was 99.65%, the PO yield was 91.83%, and the PG yield was 4.33%. Ketal (aldehyde) synthesis reaction: The above-mentioned pot material was distilled out of P0, the kettle was transfered to a four-necked bottle equipped with a stirring, thermometer, water separator, and reflux condenser, 3.15 g of cyclohexanone (the molar ratio of cyclohexanone to PG is 2), the reaction temperature was controlled to reflux and divert water to no moisture, after 2h of reaction, cooling, sampling and analysis, the catalyst was recovered by filtration, the filtrate was distilled to separate the solvent, raw material cyclohexanone, and the product cyclohexanone 1,2-propanediol ketal, the recovered catalyst and the recovered solvent propionitrile were applied to the epoxidation reaction. The conversion of PG was 98.48%, and the yield of cyclohexanone 1, 2-propanediol ketal was 90.11% (for PG). |
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