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CAS RN: 50525-27-4 | 产品编码: T1655
Tris(2,2'-bipyridyl)ruthenium(II) Chloride Hexahydrate
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产品编码 | T1655 |
纯度/分析方法 | >98.0%(T) |
分子式/分子量 | C__3__0H__2__4Cl__2N__6Ru·6H__2O = 748.62 |
外观与形状(20°C) | 固体 |
储存温度 | 室温 (15°C以下阴凉干燥处) |
储存在惰性气体下 | 存放于惰性气体之中 |
应避免的情况 | 空气 |
包装和容器 | 1G-带有塑料内管的玻璃瓶 (查看图片), 250MG-带有塑料内管的玻璃瓶 (查看图片) |
CAS RN | 50525-27-4 |
Reaxys-RN | 14615736 |
PubChem物质ID | 87577396 |
MDL编号 | MFCD00149670 |
Appearance | Orange to Amber to Dark red powder to crystal |
Purity(Precipitation Titration) | min. 98.0 % |
Water | 12.0 to 15.0 % |
水溶性 | 可溶 |
RTECS# | VM2730000 |
新化学物质备案回执号 | B1A232215734 |
监管条件代码(*) |
Used Chemicals
Procedure
Ru(bpy)3Cl2・6H2O (80.1 mg, 0.125 mmol, 2.5 mol%), caffeine (9.71 g, 50.0 mmol, 10 eq.), 4-methoxybenzenediazonium tetrafluoroborate (1.11 g, 5.00 mmol, 1.0 eq.) and formic acid (25 mL) were added to a 100 mL four-necked round bottomed flask at room temperature. The mixture was placed at a distance of 2-3 cm from Blue LED lamps. The brown solution was stirred at rt under visible light irradiation. After 14 hours of irradiation, 5% sodium bicarbonate and dichloromethane were added. The organic layer was washed with brine. Organic layer was dried over Na2SO4 and concentrated under reduced pressure to afford the crude product as a red solid (8.20 g), which was purified by column chromatography on silica gel (hexane:ethyl acetate = 80:20 - 34:66) to afford compound 1 as a pale red solid (632 mg, y. 42 %).
Experimenter’s Comments
The flask was irradiated with 40 W blue LED lamps (3 cm away, with cooling fans to keep the reaction at room temperature).
The reaction mixture was monitored by 1H NMR.
Analytical Data(Compound 1)
1H NMR (400 MHz, CDCl3); δ 7.62 (d, J = 8.7 Hz, 2H), 7.01 (d, J = 8.7 Hz, 2H), 4.02 (s, 3H), 3.86 (s, 3H), 3.61 (s, 3H), 3.41 (s, 3H).
13C NMR (101 MHz, CDCl3); δ 161.1, 155.5, 152.1, 151.7, 148.2, 130.6, 120.5, 114.3, 108.2, 55.4, 33.9, 29.8, 27.9.
Lead Reference
- Direct Arylation of N-Heteroarenes with Aryldiazonium Salts by Photoredox Catalysis in Water
Other Reference
- Room-Temperature C–H Arylation: Merger of Pd-Catalyzed C–H Functionalization and Visible-Light Photocatalysis
文章/手册
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