Preparation method of catalyst for hydrogenation reduction reaction of 2-alkylene cyclobutanone
A technology of hydrocarbyl cyclobutanone and catalyst, which is applied in the direction of catalyst activation/preparation, carbon-based compound preparation, organic compound preparation, etc. It can solve the problems of being easily destroyed, and achieve the effects of easy operation, mild reaction conditions, and easy preparation
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Embodiment 1
[0017] 1. Catalyst preparation: In an ice-water bath, mix 20 mL of ethanol solution containing sodium borohydride with a concentration of sodium borohydride of 1 mol / L, 20 mmol of selenium powder (the molar dosage is 100% of sodium borohydride) and 0.6 mmol of auxiliary agent 3 - Proselenyl-2-alanine (molar dosage is 0.03 times of sodium borohydride) is mixed, then 6 mmol of p-dibenzyl chloride (molar dosage is 30% of sodium borohydride) is added dropwise, after mixing evenly, then The mixture was heated to 45° C. with stirring to react for 24 hours. After the reaction is finished, filter and take the solid phase to obtain the selenium-containing high polymer. The solid was soaked in 0.3 mol / L palladium nitrate aqueous solution for 24 hours, filtered, washed with deionized water, and dried to obtain the catalyst.
[0018] 2. Application: Add 1 mmol 2-benzylidene cyclobutanone and 10 mg catalyst into 10 mL tetrahydrofuran, flow hydrogen at normal temperature and pressure for 1...
Embodiment 2
[0020] Other conditions are the same as in Example 1, and the activity of catalysts prepared by ethanol solutions of different concentrations of sodium borohydride is checked, and the experimental results are shown in Table 1.
[0021] Table 1 Test of activity of catalysts prepared with different concentrations of sodium borohydride
[0022] Numbering Sodium borohydride concentration (mol / L) Normal temperature and pressure hydrogenation yield 1 0.2 51 2 0.5 72 3 1.0 82 (Example 1) 4 1.5 70 5 2.0 61
[0023] From the above results, it can be seen that when the content of sodium borohydride in the ethanol solution of sodium borohydride is 1.0mol / L, the catalytic hydrogenation yield of the catalyst obtained by the reaction is the highest, reaching 82%.
Embodiment 3
[0025] Other conditions are the same as in Example 1, and the activity of the catalyst prepared by different selenium powder dosages is tested, and the experimental results are shown in Table 2.
[0026] The test of catalyst activity prepared by different selenium powder consumptions of table 2
[0027] Molar amount of selenium powder / Molar amount of sodium borohydride 50% 80% 100% 150% 200% Normal temperature and pressure hydrogenation yield / % 46 76 82 (Example 1) 80 72
[0028] As can be seen from the above results, the catalytic hydrogenation yield of the catalyst obtained when the amount of selenium powder is 100% of the molar weight of sodium borohydride is the highest, reaching 82% (Example 1).
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