A kind of preparation method and application of metal-organic three-membered cyclic compound
A cyclic compound and metal-organic technology, which is applied in the field of preparation of metal-organic ternary cyclic compounds, can solve the problems of mild reaction conditions, long reaction time and high production cost, and achieves stable chemical properties, easy mass synthesis, and good quality. The effect of reducing activity
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Embodiment 1
[0027]Step 1, 4-bromo-3-nitrotoluene (12.96g, 60mmol), pinacol diborate (18.29g, 72mmol) and potassium acetate (23.56g, 240mmol) were dissolved in 200mL dioxane, The mixture was stirred under argon atmosphere for 15 minutes. Then [1,1'-bis(diphenylphosphino)ferrocene]palladium dichloride (2.20 g, 3 mmol) was added to the mixture, the reaction temperature was 85°C, stirred for 12 hours, and then cooled to 25°C; The reacted mixture was washed with 200 mL of CH 2 Cl 2 Extract to obtain an organic phase; then dry the organic phase with anhydrous sodium sulfate, vacuum filter, retain the filtrate, and spin to dry the solvent. Petroleum ether and dichloromethane with a volume ratio of 2:1 were passed through a silica gel column to obtain 10.02 g of yellow crystals, with a yield of 63.33%; 1 H-NMR (600MHz, DMSO-d 6 ,ppm)δ8.01(s,1H),7.63(d,J=7.40Hz,1H),7.51(d,J=7.40Hz,1H),2.44(s,3H),1.33(s,12H).
[0028] Step 2, weigh the yellow crystal (5g, 19mmol) obtained in step 1 and 2-bromo...
Embodiment 2
[0036] Will Co(NO 3 ) 2 ·6H 2 O (17.46mg, 0.06mmol) and the ligand H prepared in Example 1 2 Add DPD (33.57mg, 0.04mmol) into 12mL of a mixed solvent of methanol and acetonitrile with a volume ratio of 1:1.2, then put the mixture in an oven, first heat up for 1 hour, when the temperature rises to 82°C, keep it warm for 1 hour , and then cooled down to 33°C within 15 hours. After standing at room temperature for 6 days, a dark red solid precipitated on the bottle wall, and 24.31 mg of the target compound Co-DPD was obtained with a yield of 59.92%. ESI-MS mass spectrum: m / z: 896.5069[Co 3 (DPD) 3 ] 3+ .
Embodiment 3
[0038] Co(BF 4 ) 2 ·6H 2 O (20.44mg, 0.06mmol) and the ligand H prepared in Example 1 2 DPD (33.57mg, 0.04mmol) was added to 13mL of a mixed solvent of methanol and acetonitrile with a volume ratio of 1:0.9, and then the mixture was placed in an oven, and the temperature was raised for 1 hour. When the temperature rose to 80°C, it was kept for 1 hour. , and then cooled down to 28°C within 14 hours. After standing at room temperature for 1 week, a dark red solid precipitated on the bottle wall, and 22.80 mg of the target compound Co-DPD was obtained with a yield of 56.21%. ESI-MS mass spectrum: m / z: 896.5069[Co 3 (DPD) 3 ] 3+ .
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