Volatile metal beta-ketoiminate complexes
A technology of metal complexes and complexes, applied in gold organic compounds, compounds containing elements of group 3/13 of the periodic table, compounds containing elements of group 8/9/10/18 of the periodic table, etc., can solve three Contamination of reaction chamber by alkylphosphine ligands, etc.
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Embodiment 1
[0074] Embodiment 1: synthetic H 2 NCH 2 CH 2 OSiMe 2 (C 2 h 3 )
[0075] 80.0 ml (0.57 mol) of chlorodimethylvinylsilane and 79.0 ml (0.57 mol) of triethylamine were mixed together with 2.0 liters of dry hexane and vigorously stirred at room temperature under a nitrogen atmosphere. 35.0 ml ethanolamine (0.57 mol) was slowly added over a period of 1 hour to give a white viscous slurry. The solid triethylamine hydrochloride was filtered off under nitrogen and washed with an additional 1.0 liter of dry hexane. Hexane was then distilled from the product at atmospheric pressure to yield 58.0 g (70%) of product. The NMR result of product is as follows:
[0076] 1 H NMR: (5O0MHz, C 6 D. 6 ): δ=0.15(d, 6H), δ=2.8(q, 2H), δ=3.5(t, 2H), δ=5.75(dd, 1H), δ=5.94(dq, 1H), δ=6.17 (dq, 1H).
Embodiment 2
[0077] Embodiment 2: Synthesis of MeC(O)CH 2 C(NCH 2 CH 2 OSiMe 2 (C 2 h 3 )) Me
[0078] 58.3g (0.40mol) H 2 NCH 2 CH 2 OSiMe 2 (C 2 h 3 ) was slowly added dropwise to 250 ml THF at room temperature in the presence of excess sodium sulfate and under stirring, wherein the THF contained 40 g (0.40 mol) of 2,4-pentanedione. The mixture was stirred for 4 hours, then the THF was stripped under vacuum. The residue was then distilled at 120 °C / 20 mTorr to give 35 g of the final product (43% yield). The NMR result of product is as follows:
[0079] 1 H NMR: (500MHz, C 6 D. 6 ): δ=0.15(s, 6H), δ=1.40(s, 3H), δ=2.0(s, 3H), δ=2.8(q, 2H), δ=3.27(q, 2H), δ=4.9 (s, 1H), δ=5.75(m, 1H), δ=5.95(m, 1H), δ=6.1(m, 1H).
Embodiment 3
[0080] Embodiment 3: synthetic Cu (MeC (O) CHC (NCH 2 CH 2 OSiMe 2 (C 2 h 3 ))Me)
[0081] 17.0g (0.075mol) MeC(O)CH 2 C(NCH 2 CH 2 OSiMe 2 (C 2 h 3 ))Me was dissolved in 10.0 ml of dry tetrahydrofuran (THF) solvent, and added to 100 ml of dry THF under nitrogen atmosphere in a stirring state for 1 hour, wherein the THF contained 2.5 g (40% excess, 1.04 mol ) sodium hydride, then stirred overnight at room temperature. The mixture was filtered under nitrogen and then slowly added to 7.5 g (0.075 mol) of copper(I) chloride stirred in 10 ml of dry THF at 0° C. under nitrogen over a period of 1 hour and the mixture was subsequently heated to room temperature and stirred overnight. The THF was then stripped off under vacuum and added to 500 ml of dry deoxygenated hexane and stirred for 10 minutes before filtration. After stripping the hexane under vacuum, the crude product was obtained as light blue crystals in a yield of 15.8 g (73%). After sublimation at 20 mTorr an...
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