Ternary sulfonimine transition metal salt and synthesis method thereof
A technology of transition metal salts and sulfonimides, applied in the field of trivalent transition metal salts of ternary sulfonimides and their synthesis, achieving the effects of simple synthesis methods, good catalytic activity and stereoselectivity
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Embodiment 1
[0023] Embodiment 1: the synthesis of ternary fluorine-containing sulfonamide nitrogen super acid lanthanum
[0024]
[0025] (1) Synthesis of ternary fluorine-containing sulfonamide nitrogen superacid
[0026] Synthetic steps
[0027]
[0028] Take 0.0081 moles of IBSC dissolved in 5ml of CH 3 NO 2 The solvent was poured into a 100ml three-neck flask with a reflux condenser of a bubbler and a drying tube. Take 0.0162 moles of perfluorosulfonamide and use 25ml of solvent to obtain a colorless and transparent solution. First pass argon gas to drive out the air and then stop. At a bath temperature of 80°C and magnetic stirring, the perfluorosulfonamide solution was added to obtain a pale yellow solution. During the reaction, bubbles were generated in the bubbler, and a white solid precipitate was gradually produced. After 48 hours, almost no bubbles emerged, and the reaction was stopped. After filtering in a drying oven, the obtained solid was dried under reduced pr...
Embodiment 2
[0030] Dissolve 0.0108 moles of IBSC in 5ml of CH 3 CN solvent, take 0.0216 moles of perfluorosulfonamide, under the same test conditions as above, 1.59 grams of solid can be obtained, and the yield is 20%.
[0031] Structure Characterization:
[0032] FT-IR: 3120cm -1 There is a single N-H stretching vibration, with C 4 f 9 SO 2 NH 2 The comparison found that the characteristic peaks (946, 800, 655, 500cm) of many raw materials in the fingerprint area -1 )disappear
[0033] 1 HNMR: (TMS internal standard, DMSO-d 6 For solvent) there are three equal-area peaks at 6.46, 7.04, and 7.60ppm, which are triplets formed by H-N coupling, 1 J HN = 56Hz. No C in the spectrum 4 f 9 SO 2 NH 2 H peak (7.52ppm).
[0034] 19 F NMR: (CFCl 3 Internal standard, DMSO-d 6 is the solvent) has the following peaks: -81.0ppm triplet (3F); -113.9ppm triplet (2F); -121.0ppmmultipeak (2F); -124.5ppm triplet (2F).
[0035] Melting point.: 156.4-163.5°C
[0036] Elemental analysis: C...
Embodiment 3
[0041] Example 3: Diels-Alder reaction catalyzed by aliphatic fluorine-containing ternary sulfonylimide nitrogen salt
[0042]
[0043] Add 5.59mmol methyl vinyl ketone, 8.99mmol cyclopentadiene, 1mmol% of the above-mentioned salt as a catalyst, and 50mL dichloromethane into a 100mL round bottom flask in sequence, and react under electromagnetic stirring at room temperature. The reaction process was tracked by gas chromatography, and the result showed that the reaction 40 was completed. The solvent was evaporated, and the initial product was washed with water until neutral, and then recrystallized with petroleum ether. After filtering and drying, 5.5 mmol of the product was obtained with a yield of 98%.
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