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Three-Dimensional Printing in Catalysis

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    S1 Supporting Information Three - Dimensional Printing in Catalysis: Combining 3D Heterogeneous Copper and Palladium Catalysts for Multicatalytic Multicomponent Reactions   Antonio S. Díaz-Marta, 1,‡  Carmen R. Tubío, 2,‡  Carlos Carbajales, 1  Carmen Fernández, 1  Luz Escalante, 1  Eddy Sotelo, 1,4  Francisco Guitián, 2  V. Laura Barrio, 3  Alvaro Gil* ,2  and Alberto Coelho* ,1,4   1 Centro Singular de Investigación en Química Biolóxica e Materiáis Moleculares (CIQUS) . Universidade de Santiago de Compostela, E - 15782, Santiago de Compostela, Spain   2 Instituto de Cerámica, Universidade de Santiago de Compostela, E - 15782, Santiago de Compostela, Spain   3 Escuela de Ingeniería, Universidad del País Vasco , Alameda Urquijo s/n, E -   48013, Bilbao, Spain   4 Departamento de Química Orgánica, Facultad de Fa rmacia. Universidade de Santiago de Compostela, E - 15782, Santiago de Compostela, Spain   alvaro.gil@usc.es   albertojose.coelho@usc.es   Table of contents: page 1.   SEM images showing the rod surface of the 3D-SiO 2 -APTS-Cu and 3D-SiO 2 -AAPTS-Pd catalyst rod surface before and after carrying out the catalytic reactions………………………………………………………….…S2 2.   Survey XPS spectra of 3D-SiO 2 -APTS-Cu and 3D-SiO 2 -AAPTS-Pd monoliths............................................................................................................S3 3.   Three Phase Tests for 3D-SiO 2 -APTS-Cu and 3D-SiO 2 -AAPTS-Pd ……...S4 4.   NMR spectroscopic data and spectra of the related compounds…………..S8    S2 1. SEM images showing the rod surface of the 3D-SiO 2 -APTS-Cu and 3D-SiO 2 -AAPTS-Pd catalyst rod surface before and after carrying out the catalytic reactions (scale bar 100 ! m). Figure S1    S3 2- Survey XPS spectra of SiO 2 -APTS-Cu and SiO 2 -AAPTS-Pd monoliths. a) SiO 2 -APTS-Cu b) SiO 2 -AAPTS-Pd Figure S2a,b    S4 3- Three Phase Test for 3D-SiO 2 -APTS-Cu: Synthesis of the supported reagent II (Scheme S1):  To a 50 mL glass fritted reaction vessel was added Wang resin (4.0 g, 1.25 mmol/g, 5.0 mmol). The resin was firstly washed with dry dichloromethane (2 x 30 mL) and then suspended in dry dichloromethane (30 mL). To the resin slurry was added diethylisopropylamine (30 mmol) and the vessel submitted to orbital stirring for 5 minutes before 4-(chloromethyl)benzoyl chloride (25 mmol) was added in one portion. The resulting slurry was stirred for 24 hours at room temperature. The resin was filtered, successively washed with dichloromethane (2 x 40 mL), methanol (2 x 30mL) and tetrahydrofurane (3 x 40 mL) and dried in vacuum for 8 h at room temperature. Tetrabuthylammonium fluoride (50 mmol) and trimethylsilyl azide (50 mmol) were added to the resin in dichloromethane (15 mL) and the resulting slurry was stirred for 24 hours at room temperature. The resin was filtered, successively washed with tetrahydrofurane (3 x 40 mL), methanol (2 x 30mL) and dichloromethane (3x 40 mL) and dried in vacuum for 8 h at room temperature. Scheme S1 Three Phase Test experiment (Scheme S2): Two parallel experiments were  performed, experiments 1 and 2.  Experiment 1 (control):  To the supported benzyl azide II (1.0 g, 1.25 mmol) in DMF (10 mL) were added phenylacetylene (10 mmol), DIPEA (10 mmol) and CuI (0.05 mmol) and the resulting slurry was submitted to orbital stirring for 48 hours. The resin was filtered, successively washed with dichloromethane (2 x 20 mL), methanol (2 x 15 mL) and dichloromethane (3 x 20 mL) and dried in vacuum for 8 h at room temperature. To the previously obtained resin suspended in dichloromethane (15 mL) was added trifluoroacetic acid (3.0 mL) and the resulting slurry stirred at room temperature for 2 hours, then filtered and washed with dichloromethane (3 x 15 mL). The combined OHClOClOOClDIEA/CH 2 Cl 2 OON 3 TMS-N 3 TBAF I II Wang resin

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