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Volumn , Issue 1, 2007, Pages 131-135

Simple and efficient microwave-assisted hydrogenation reactions at moderate temperature and pressure

Author keywords

Hydrog nations; Microwave; Palladium; Reductions; Simultaneous cooling

Indexed keywords

HYDROGEN; NITROBENZENE DERIVATIVE; PALLADIUM; PHENYLACETYLENE;

ARTICLE; CATALYST; CHEMICAL ANALYSIS; CHEMICAL REACTION; COOLING; HYDROGENATION; MICROWAVE IRRADIATION; PRESSURE; REACTION ANALYSIS; TEMPERATURE;

EID: 33846413209 PISSN: 09365214 EISSN: None Source Type: Journal
DOI: 10.1055/s-2006-958428 Document Type: Article

Times cited : (94)

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- Experimental Set-up. All reactions were performed with a CEM Discover single mode microwave reactor equipped with a 300 W power source. A 10 mL fiber optic accessory was equipped with a gas inlet to allow introduction of hydrogen gas to the reaction vessel, and each of the reactions was performed in a CEM 10 mL microwave reaction vial. All temperature measurements were performed with a fiber optic probe, and 2 mL of solvent was used for each reaction to ensure ample submersion of the fiber optic probe. General Procedure. To a solution of trans,trans-1,4-diphenyl-1,3-butadiene (1, 103 mg, 0.500 mmol) in 2.0 mL of EtOAc was added Pd/C 10 wt, 5 mg, 0.005 mmol, The reaction vessel was purged three times with hydrogen, charged to 50 psi, and then closed off to the source of hydrogen. The reaction was heated under microwave irradiation to 80 °C with 100 W of power and held for 5 min. Upon cooling to ambient temperature, the reaction mixture was filtered through Ce
- 3): δ = 142.66, 128.53, 128.38, 125.77, 35.93, 31.20. Characterization data is consistent with that of commercially available material.

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- Isolated yields were difficult due to the low volatility of the products.

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