Maximum quantity allowed is 999
CAS RN: 13965-03-2 | 产品编码: B1667
Bis(triphenylphosphine)palladium(II) Dichloride
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产品编码 | B1667 |
纯度/分析方法 | >98.0%(T) |
分子式/分子量 | C__3__6H__3__0Cl__2P__2Pd = 701.90 |
外观与形状(20°C) | 固体 |
储存温度 | 冷藏 (0-10°C) |
储存在惰性气体下 | 存放于惰性气体之中 |
应避免的情况 | 湿气 (分解),加热 |
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 | 13965-03-2 |
Reaxys-RN | 13172189 |
PubChem物质ID | 87564568 |
SDBS (AIST Spectral DB) | 27199 |
MDL编号 | MFCD00009593 |
Appearance | Light yellow to Brown powder to crystal |
Purity(Chelometric Titration) | min. 98.0 % |
NMR | confirm to structure |
新化学物质备案回执号 | B1A232215381 |
监管条件代码(*) |
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Used Chemicals
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Procedure
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To a two-necked flask was charged with iodobenzene (1.09 mL, 9.80 mmol, 1.0 equiv.), ethynylbenzene (1.18 mL, 10.7 mmol, 1.1 equiv.), bis(triphenylphosphine)palladium(II) dichloride (137 mg, 0.195 mmol 2.0 mol%), copper(I) iodide (40 mg, 0.210 mmol, 2.1 mol%), tetrahydrofuran anhydrous (40 mL), triethylamine (1.90 mL, 14.7 mmol, 1.5 equiv.) under nitrogen atmosphere. The mixture was stirred at room temperature for 1.5 h. The reaction mixture was quenched with water (20 mL). The organic layer was washed with brine (10 mL), dried over Na2SO4 and then concentrated under reduce pressure. The crude was purified by column chromatography on silica gel (hexane) to afford diphenylacetylene as a white powder (1.70 g, 97 %).
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Experimenter’s Comments
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The reaction mixture was monitored by GC.
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Analytical Data
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Diphenylacetylene
1H NMR (400 MHz, CDCl3); δ 7.51-7.54 (m, 4H), 7.31-7.35 (m, 6H).
13C NMR (101 MHz, CDCl3); δ 131.6, 128.3, 128.2, 123.2, 89.3.
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Other References
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- A convenient synthesis of acetylenes: catalytic substitutions of acetylenic hydrogen with bromoalkenes, iodoarenes and bromopyridines
References
- One-Pot Procedure for the Synthesis of Unsymmetrical Diarylalkynes
文章/手册
[研究论文] One-pot Procedure for the Synthesis of Unsymmetrical Diarylalkynes
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