Metal complexes
A technology of compounds and general formulas, which is applied in the field of preparing the metal complexes, and can solve problems such as increased solubility of complexes
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Embodiment 1
[0214] Preparation of Compound III
[0215] The synthetic method of preparing compound III:
[0216]
[0217] With the compound I of 15.0g (16.8mmol), the compound II of 38.1g (134.6mmol) and the K 3 PO 4 Suspended in 2100ml of p-xylene. 117mg (0.5mmol) of Pd(OAc) 2 and 6.7 ml of a 1M solution of tri-tert-butylphosphine were added to the suspension. The reaction mixture was heated at reflux for 27 hours. After cooling, the organic phase is separated off, washed three times with 300 ml of water and then evaporated to dryness. The residue was recrystallized from DMSO and finally dried under reduced pressure. The yield is 8.5 g (6.7 mmol), corresponding to 34% of theory.
Embodiment 2
[0219] Preparation of compound V
[0220] Synthetic steps for preparing compound V:
[0221]
[0222] 17.0 g (190 mmol) of compound I, 74.2 g (479 mmol) of compound IV, 27.2 g (182 mmol) of potassium carbonate were suspended in 350 ml of toluene and 300 ml of water. 211 mg (0.18 mmol) of tetrakis(triphenylphosphine)palladium(0) were added to the suspension, and the reaction mixture was heated under reflux for 24 hours. After cooling, the organic phase was separated off, washed three times with 200 ml of water, dried over sodium sulfate and then evaporated to dryness. The residue was washed with ethanol, recrystallized from DMSO and finally dried under reduced pressure. The yield is 21.9 g (11.2 mmol), corresponding to 58.7% of theory.
Embodiment 3
[0224] Preparation of compound VIII
[0225]
[0226] a) Synthesis of Compound VII
[0227] Suspend 22.4g (37.7mmol) of compound VI, 10.5g (41.5mmol) of bispinacolate diboron, and 9.8g (100mmol) of potassium acetate in 300ml di in alkane. 0.9 g (1.1 mmol) of 1,1-bis(diphenylphosphino)ferrocenedichloropalladium(II)*DCM were added to the suspension and the reaction mixture was heated at reflux for 8 hours . After cooling, 200 ml of ethyl acetate and 400 ml of water were added and the organic phase was separated off, washed three times with 300 ml of water, dried using sodium sulfate and then evaporated to dryness. The residue is washed with ethanol, recrystallized from ethyl acetate and finally dried under reduced pressure. The yield is 19.3 g (30 mmol), corresponding to 79.8% of theory.
[0228] b) Synthesis of Compound VIII
[0229] 27.2 g (30.5 mmol) of compound I, 118.7 g (185.3 mmol) of compound VII, 30.3 g (286.6 mmol) of potassium carbonate were suspended in 700...
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